Water → Benzyl 4-mercapto-2-methylbutan-2-ylcarbamate

HRID 1770677ノート

反応式

HRID 1770677 の反応式
C(=O)([S:3][CH2:4][CH2:5][C:6]([NH:9][C:10]([O:12][CH2:13][C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)=[O:11])([CH3:8])[CH3:7])C.[OH-].[Na+].O>CO>[SH:3][CH2:4][CH2:5][C:6]([NH:9][C:10](=[O:11])[O:12][CH2:13][C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)([CH3:8])[CH3:7]

参加物

5

反応物 3

HCID 962WaterHCID 14798Sodium HydroxideHCID 86665510HCID 86665510、化合物

生成物 1

HCID 86665509Benzyl 4-mercapto-2-methylbutan-2-ylcarbamate

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a solution of S-3-(benzyloxycarbonylamino)-3-methylbutyl ethanethioate (1.52 g, 5.14 mmol, prepared as described in WO 2008/083347) in methanol (25 ml) was added 5.0 M NaOH in H2O (3.3 ml, 16.5 mmol). The solution was stirred for 1 hour, concentrated in vacuo, and the residue suspended in 100 ml 1M H3PO4, extracted with 5×50 ml ethyl acetate, the organic layers combined and washed once with 100 ml saturated NaCl, dried on MgSO4, and concentrated in vacuo. The reaction product was used in the next step without further purification.

後処理

  1. concentrationconcentrated in vacuo
  2. extractionextracted with 5×50 ml ethyl acetate
  3. washwashed once with 100 ml saturated NaCl
  4. customdried on MgSO4
  5. concentrationconcentrated in vacuo
  6. customThe reaction product was used in the next step without further purification

出典と根拠

ORDレコード
ord-2660d65411074ba49bc0faef8570bb73
出典データセット
uspto-grants-2016_02
特許番号
US09248117B2

反応ノート

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