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

Potassium Carbonate → tert-Butyl 4-{[({[(2S)-4-(3,4-dichlorobenzyl)morpholin-2-yl]methyl}amino)carbonyl]amino}butanoate

HRID 1371389
ノート
印刷プレビュー

反応式

HRID 1371389 の反応式
Cl.[C:2]([O:6][C:7](=[O:12])[CH2:8][CH2:9][CH2:10][NH2:11])([CH3:5])([CH3:4])[CH3:3].[Cl:13][C:14]1[CH:15]=[C:16]([CH:38]=[CH:39][C:40]=1[Cl:41])[CH2:17][N:18]1[CH2:23][CH2:22][O:21][C@@H:20]([CH2:24][NH:25][C:26](=O)[O:27]C2C=CC([N+]([O-])=O)=CC=2)[CH2:19]1.C(N(CC)C(C)C)(C)C.C(=O)([O-])[O-].[K+].[K+]>ClCCl>[Cl:13][C:14]1[CH:15]=[C:16]([CH:38]=[CH:39][C:40]=1[Cl:41])[CH2:17][N:18]1[CH2:23][CH2:22][O:21][C@@H:20]([CH2:24][NH:25][C:26]([NH:11][CH2:10][CH2:9][CH2:8][C:7]([O:6][C:2]([CH3:5])([CH3:3])[CH3:4])=[O:12])=[O:27])[CH2:19]1
参加物反応条件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 11430Potassium CarbonateHCID 81531DiisopropylethylamineHCID 117750244-Nitrophenyl [(2S)-4-(3,4-dichlorobenzyl)morpholin-2-yl]methylcarbamateHCID 24750478Tert-butyl 4-aminobutanoate hydrochloride

生成物 1

HCID 86760343tert-Butyl 4-{[({[(2S)-4-(3,4-dichlorobenzyl)morpholin-2-yl]methyl}amino)carbonyl]amino}butanoate収率 75%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
22 °C

実験手順

4-Aminobutyric acid tert-butyl ester hydrochloride (0.235 g) was added to a stirred solution of Intermediate 13 (0.440 g) and N,N-diisopropylethylamine (0.42 ml) in dry dichloromethane (20 ml) under nitrogen, and the mixture was stirred at 22° C. for 18 h. The mixture was treated with saturated aqueous potassium carbonate (20 ml) and stirred for 5 min. The layers were separated and the organic layer applied to a silica gel cartridge (10 g Varian Bond Elut). Elution with dichloromethane, ether, ethyl acetate, and acetone gave the crude product (0.357 g). Further purification by chromatography on silica gel (10 g Varian Bond Elut cartridge), eluting with dichloromethane (1 column volume), ether (4 column volumes) and ethyl acetate (8 column volumes) gave the title compound as a gum (0.345 g).

後処理

  1. stirringstirred for 5 min
  2. customThe layers were separated
  3. washElution with dichloromethane, ether, ethyl acetate, and acetone
  4. customgave the crude product (0.357 g)
  5. customFurther purification by chromatography on silica gel (10 g Varian Bond Elut cartridge)
  6. washeluting with dichloromethane (1 column volume), ether (4 column volumes) and ethyl acetate (8 column volumes)

出典と根拠

ORDレコード
ord-244ca70a9aa544318514685e5b6668d6
出典データセット
uspto-grants-2007_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07157457B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート