溶剂的化学位移(氢谱)

Notes

Table1.

proton

solventresidualpeakH2O

aceticacidacetoneacetonitrilebenzene

tert-butylalcoholtert-butylmethyletherBHTb

multssssssssssssssssst,7q,7mmssssssssssst,7q,7dsc,dsq,7t,7sq,7t,7sembrstmd,9.5shsc,hst,7md,6sep,6mmmsmmsmmt,7q,7

CDCl37.261.562.102.172.107.361.281.193.226.985.012.271.437.261.433.735.301.213.483.653.573.393.403.552.093.022.948.022.962.882.623.711.253.721.322.054.121.262.142.461.063.760.861.260.881.262.653.491.094.330.881.271.224.048.627.297.680.071.853.762.367.177.251.032.53

1H

.Chem.,Vol.62,No.21,19977513

NMRData

(CD3)2SO2.503.33a1.912.092.077.371.114.191.113.086.876.652.181.368.321.403.905.761.093.383.513.383.243.243.431.962.942.787.952.892.732.543.571.063.444.631.994.031.172.072.430.913.340.861.252.533.164.014.420.861.271.043.788.587.397.791.763.602.307.187.250.932.43

C6D67.160.401.551.551.557.151.051.551.073.047.054.792.241.386.151.402.904.271.113.263.463.343.113.123.331.602.572.057.632.361.861.683.350.963.341.653.890.921.581.810.853.410.921.360.891.242.403.072.940.871.230.953.678.536.666.980.291.403.572.117.027.130.962.40

CD3CN1.942.131.962.081.967.371.162.181.143.136.975.202.221.397.581.443.815.441.123.423.533.453.293.283.451.972.962.837.922.892.772.503.601.123.542.471.974.061.202.062.430.963.510.861.270.891.282.573.282.164.310.891.291.093.878.577.337.730.081.803.642.337.1-7.37.1-7.30.962.45

CD3OD3.314.871.992.152.037.331.401.153.206.922.211.407.901.453.785.491.183.493.613.583.353.353.522.073.312.927.972.992.862.653.661.193.602.014.091.242.122.501.013.590.881.290.901.292.643.344.340.901.291.503.928.537.447.850.101.873.712.327.167.161.052.58

D2O4.792.082.222.061.241.213.22

(CD3)2CO2.052.84a1.962.092.057.361.181.133.136.962.221.418.021.433.875.631.113.413.563.473.283.283.461.973.002.837.962.942.782.523.591.123.573.391.974.051.202.072.450.963.280.871.290.881.282.593.313.124.430.881.271.103.908.587.357.760.131.793.632.327.1-7.27.1-7.20.962.45

chloroformcyclohexane

1,2-dichloroethanedichloromethanediethyletherdiglyme

1,2-dimethoxyethanedimethylacetamidedimethylformamidedimethylsulfoxidedioxaneethanolethylacetateethylmethylketoneethyleneglycol“grease”fn-hexaneHMPAgmethanolnitromethanen-pentane2-propanolpyridinesiliconegreaseitetrahydrofurantoluenetriethylamine

a

CH3CH3CH3CHCH3OHcCCH3OCH3ArHOHcArCH3

ArC(CH3)3CHCH2CH2CH2CH3CH2CH2CH2OCH3CH3CH2

CH3CONCH3NCH3CHCH3CH3CH3CH2CH3CH2OHCH3COCH2CH3CH2CH3CH3COCH2CH3CH2CH3CHCH3CH2CH3CH2CH3CH3OHCH3CH3CH2CH3CHCH(2)CH(3)CH(4)CH3CH2CH2OCH3

CH(o/p)CH(m)CH3CH2

1.173.563.673.613.373.373.602.083.062.907.923.012.852.713.751.173.652.074.141.242.193.181.263.65

2.613.344.401.174.028.527.457.871.883.74

0.992.57

InthesesolventstheintermolecularrateofexchangeisslowenoughthatapeakduetoHDOisusuallyalsoobserved;itappearsat2.81and3.30ppminacetoneandDMSO,respectively.Intheformersolvent,itisoftenseenasa1:1:1triplet,with2JH,D)1Hz.b2,6-Dimethyl-4-tert-butylphenol.cThesignalsfromexchangeableprotonswerenotalwaysidentified.dInsomecases(seenotea),thecouplinginteractionbetweentheCH2andtheOHprotonsmaybeobserved(J)5Hz).eInCD3CN,theOHprotonwasseenasamultipletatδ2.69,andextracouplingwasalsoapparentonthemethylenepeak.fLong-chain,linearaliphatichydrocarbons.TheirsolubilityinDMSOwastoolowtogivevisiblepeaks.gHexamethylphosphoramide.hInsomecases(seenotesa,d),thecouplinginteractionbetweentheCH3andtheOHprotonsmaybeobserved(J)5.5Hz).iPoly(dimethylsiloxane).ItssolubilityinDMSOwastoolowtogivevisiblepeaks.

showtheirdegreeofvariability.Occasionally,inordertodistinguishbetweenpeakswhoseassignmentwasambiguous,afurther1-2µLofaspecificsubstratewereaddedandthespectrarunagain.

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