Methyl iodide → Benzyl 1,1-dimethyl-2-(methylthio)ethylcarbamate

HRID 2061056노트

반응식

HRID 2061056 반응식
[SH:1][CH2:2][C:3]([NH:6][C:7](=[O:16])[O:8][CH2:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)([CH3:5])[CH3:4].[CH3:17]I>CO>[CH3:4][C:3]([NH:6][C:7](=[O:16])[O:8][CH2:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)([CH3:5])[CH2:2][S:1][CH3:17]

참가 물질

4

반응물 2

HCID 6328Methyl iodideHCID 59614731Benzyl 1-mercapto-2-methylpropan-2-ylcarbamate

생성물 1

HCID 60134425Benzyl 1,1-dimethyl-2-(methylthio)ethylcarbamate수율 65%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a pressure tube was added a solution of benzyl 1-mercapto-2-methylpropan-2-ylcarbamate in methanol (5 mL), TEA (2.35 mL, 1 equiv) and methyl iodide (1.05 mL, 1 equiv). The tube was sealed and the reaction stirred for 17 h. The solvent was removed in vacuo and the crude material was purified on an ISCO purification system. The desired fractions were pooled and concentrated under reduced pressure to give a pale yellow oil (2.78 g, 65%). 1H NMR (CDCl3, 400 MHz): δ 1.41 (s, 6H), 2.51 (s, 2H), 2.98 (s, 2 H). LRMS (ESI+) for C13H19NO2S (253.1); Found: 254 (MH+).

후처리

  1. customThe tube was sealed
  2. customThe solvent was removed in vacuo
  3. customthe crude material was purified on an ISCO purification system
  4. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-5a0ca889ea0c462fbc4c09bc093cff08
출처 데이터셋
uspto-grants-2012_10
특허 번호
US08278482B2

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