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

Water → 5-[N-(N-t-butoxycarbonylglycyl)amino]-2-phenyl-1,3,4,5-tetrahydrobenz[cd]indole

HRID 1637268
ノート
印刷プレビュー

反応式

HRID 1637268 の反応式
[NH2:1][CH:2]1[C:12]2[C:13]3[C:5](=[C:6]([C:14]4[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=4)[NH:7][C:8]=3[CH:9]=[CH:10][CH:11]=2)[CH2:4][CH2:3]1.[C:20]([O:24][C:25]([NH:27][CH2:28][C:29](O)=[O:30])=[O:26])([CH3:23])([CH3:22])[CH3:21].ClC(Cl)CCCCCN=C=N.O>C(Cl)Cl>[C:20]([O:24][C:25]([NH:27][CH2:28][C:29]([NH:1][CH:2]1[C:12]2[C:13]3[C:5](=[C:6]([C:14]4[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=4)[NH:7][C:8]=3[CH:9]=[CH:10][CH:11]=2)[CH2:4][CH2:3]1)=[O:30])=[O:26])([CH3:23])([CH3:22])[CH3:21]
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 962WaterHCID 78288N-(tert-butoxycarbonyl)glycineHCID 101988185-Amino-2-phenyl-1,3,4,5-tetrahydrobenz[cd]indoleHCID 71510291Dichlorohexylcarbodiimide

生成物 1

HCID 193482985-[N-(N-t-butoxycarbonylglycyl)amino]-2-phenyl-1,3,4,5-tetrahydrobenz[cd]indole収率 143.9%

試薬・触媒・溶媒 1

HCID 6344
Dichloromethane
溶媒

実験手順

A portion (200 mg) of the compound obtained in Example 81 and N-t-butoxycarbonylglycine (170 mg) were suspended in methylene chloride (15 ml) and to the suspension was added dichlorohexylcarbodiimide (216 mg) under cooling with ice. The mixture was stirred for 1 hour at room temperature. To the reaction mixture was added water, followed by extraction with ethyl acetate. The organic layer was washed with water and saturated aqueous solution of sodium chloride and dried over anhydrous sodium sulfate. Then, the solvent was distilled off under reduced pressure to yield the titled compound (470 mg) as a crude yellow solid. The compound was used in the subsequent reaction without further purification.

後処理

  1. temperatureunder cooling with ice
  2. extractionfollowed by extraction with ethyl acetate
  3. washThe organic layer was washed with water and saturated aqueous solution of sodium chloride
  4. dry with materialdried over anhydrous sodium sulfate
  5. distillationThen, the solvent was distilled off under reduced pressure

出典と根拠

ORDレコード
ord-dcc4a09ac9b04152b0917aa97b9017e5
出典データセット
uspto-grants-2000_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06040331

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