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

HRID 2061056ノート

反応式

HRID 2061056 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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+).

後処理

  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

出典と根拠

ORDレコード
ord-5a0ca889ea0c462fbc4c09bc093cff08
出典データセット
uspto-grants-2012_10
特許番号
US08278482B2

反応ノート

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