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1-Hydroxybenzotriazole → (6S)-6-(5-chloro-2-methoxybenzyl)-1-(2,4,6-trimethoxybenzyl)-1,4-diazepan-2,5-dione

HRID 554828
ノート
印刷プレビュー

反応式

HRID 554828 の反応式
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([O:32][CH3:33])=[C:6]([CH:31]=1)[CH2:7][C@@H:8]([CH2:16][NH:17][CH2:18][C:19]1[C:24]([O:25][CH3:26])=[CH:23][C:22]([O:27][CH3:28])=[CH:21][C:20]=1[O:29][CH3:30])[C:9]([NH:11][CH2:12][C:13]([OH:15])=O)=[O:10].ON1C2C=CC=CC=2N=N1.Cl.CN(C)CCCN=C=NCC>C(#N)C>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([O:32][CH3:33])=[C:6]([CH:31]=1)[CH2:7][C@H:8]1[CH2:16][N:17]([CH2:18][C:19]2[C:24]([O:25][CH3:26])=[CH:23][C:22]([O:27][CH3:28])=[CH:21][C:20]=2[O:29][CH3:30])[C:13](=[O:15])[CH2:12][NH:11][C:9]1=[O:10]
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

5

反応物 3

HCID 757711-HydroxybenzotriazoleHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 67460156HCID 67460156、化合物

生成物 1

HCID 66935303(6S)-6-(5-chloro-2-methoxybenzyl)-1-(2,4,6-trimethoxybenzyl)-1,4-diazepan-2,5-dione

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

反応条件

温度
40 °C

実験手順

To a solution of N-{(2S)-2-(5-chloro-2-methoxybenzyl)-3-[(2,4,6-trimethoxybenzyl)amino]propanoyl}glycine (1g) in acetonitrile (30 ml), 1-hydroxy benzotriazole (421 mg) was added at room temperature. The mixture was stirred at 40° C. for 20 minutes, then N-(3-dimethylaminopropyl)-N′-ethylcarbodiimide hydrochloride (598 mg) was added to the reaction solution, and the mixture was stirred for 2 hours. After the reaction solution was concentrated in vacuo, toluene was added to the obtained residue, and the resulting mixture was washed with 6% aqueous sodium bicarbonate and saturated brine. The organic layer was concentrated in vacuo, then the obtained residue was purified by silica gel column chromatography to obtain the title compound (894 mg) as a colorless crystal.

後処理

  1. stirringthe mixture was stirred for 2 hours
  2. concentrationAfter the reaction solution was concentrated in vacuo, toluene
  3. additionwas added to the obtained residue
  4. washthe resulting mixture was washed with 6% aqueous sodium bicarbonate and saturated brine
  5. concentrationThe organic layer was concentrated in vacuo
  6. customthe obtained residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-c73109fc85b946e7971aeebbc131558b
出典データセット
uspto-grants-2011_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08049006B2

反応ノート

読み込み中…

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