ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Benzyl chloroformate → Nalphabenzyloxycarbonyl-DL-methionine amide

HRID 2270884
ノート
印刷プレビュー

反応式

HRID 2270884 の反応式
[CH2:1]([O:8][C:9](Cl)=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[NH2:12][CH:13]([C:18]([NH2:20])=[O:19])[CH2:14][CH2:15][S:16][CH3:17].[OH-].[Na+].CC(OC)(C)C>O>[CH2:1]([O:8][C:9]([NH:12][CH:13]([C:18]([NH2:20])=[O:19])[CH2:14][CH2:15][S:16][CH3:17])=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 10387Benzyl chloroformateHCID 14798Sodium HydroxideHCID 15413tert-Butyl methyl etherHCID 5687422-Amino-4-(methylthio)butanamide

生成物 1

HCID 3359717Nalphabenzyloxycarbonyl-DL-methionine amide収率 69%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

51 ml benzyloxycarbonyl chloride was dripped into a solution of 50 g (0.34 mole) DL-methionine amide in 200 ml water at 5-20° C., during which the pH was maintained at 7-9 with sodium hydroxide solution. A slimy precipitate formed immediately which became finely crystalline upon the addition of 200 ml MTBE. After the end of the addition the mixture was agitated 30 min further at room temperature. The precipitated, colorless crystals were then filtered off, washed with a little MTBE and recrystallized out of 700 ml toluene. After filtering off, washing with toluene and drying, 67 g (69%) Nαbenzyloxycarbonyl-DL-methionine amide with a melting point of 120-122° C. was obtained.

後処理

  1. customA slimy precipitate formed immediately which
  2. additionAfter the end of the addition the mixture
  3. filtrationThe precipitated, colorless crystals were then filtered off
  4. washwashed with a little MTBE
  5. customrecrystallized out of 700 ml toluene
  6. filtrationAfter filtering off
  7. washwashing with toluene
  8. customdrying

出典と根拠

ORDレコード
ord-7f17bed410f1416485389579c640c7c4
出典データセット
uspto-grants-2001_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06333176B1

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート