1-Hydroxybenzotriazole → HCID 57901813、化合物

HRID 1851428ノート

反応式

HRID 1851428 の反応式
[S:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[S:6]([NH:9][C:10]1[CH:11]=[CH:12][CH:13]=[C:14]2[C:18]=1[NH:17][C:16]([C:19]([OH:21])=O)=[CH:15]2)(=[O:8])=[O:7].Br.[Br:23][CH2:24][CH2:25][NH2:26].N1(O)C2C=CC=CC=2N=N1.Cl.CN(C)CCCN=C=NCC>O.CN(C)C=O.C(N(CC)CC)C>[Br:23][CH2:24][CH2:25][NH:26][C:19]([C:16]1[NH:17][C:18]2[C:14]([CH:15]=1)=[CH:13][CH:12]=[CH:11][C:10]=2[NH:9][S:6]([C:2]1[S:1][CH:5]=[CH:4][CH:3]=1)(=[O:7])=[O:8])=[O:21]

参加物

8

反応物 4

HCID 757711-HydroxybenzotriazoleHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 27742172-Bromoethylamine hydrobromideHCID 57476168HCID 57476168、化合物

生成物 1

HCID 57901813HCID 57901813、化合物収率 37.6%

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒HCID 8471Triethylamine溶媒

実験手順

To a mixture of 7-[(2-thienylsulfonyl)amino]-1H-indole-2-carboxylic acid (0.70 g), (2-bromoethyl)amine hydrobromide (0.49 g), 1H-1,2,3-benzotriazol-1-ol (0.32 g), triethylamine (0.34 mL) and N,N-dimethylformamide (20 mL) was added N-[3-(dimethylamino)propyl]-N′-ethylcarbodiimide hydrochloride (0.46 g) at 0° C., and the mixture was stirred at room temperature overnight. Water was added to the reaction mixture, and the obtained crystals were filtrated, washed with water and dried to give the title compound (0.35 g, 37%) as colorless crystals. melting point 218-219° C. (decomposition).

後処理

  1. filtrationthe obtained crystals were filtrated
  2. washwashed with water
  3. customdried

出典と根拠

ORDレコード
ord-92f51ad10fa34136a28bc8698b665246
出典データセット
uspto-grants-2015_02
特許番号
US08957070B2

反応ノート

読み込み中…