Tributylamine → HCID 178437917、化合物

HRID 68695

反応式

HRID 68695 の反応式
Cl.[CH2:2]([C:4]1[C:12]2[C:7](=[CH:8][C:9]([NH2:13])=[CH:10][CH:11]=2)[N:6]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[N:5]=1)[CH3:3].C(N(CCCC)CCCC)CCC.[NH:33]1[C:37]2[CH:38]=[CH:39][C:40]([C:42](O)=[O:43])=[CH:41][C:36]=2[N:35]=[CH:34]1.[I-].ClC1C=CC=C[N+]=1C>CN(C)C=O>[CH2:2]([C:4]1[C:12]2[C:7](=[CH:8][C:9]([NH:13][C:42]([C:40]3[CH:39]=[CH:38][C:37]4[NH:33][CH:34]=[N:35][C:36]=4[CH:41]=3)=[O:43])=[CH:10][CH:11]=2)[N:6]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[N:5]=1)[CH3:3]

参加物

6

反応物 4

HCID 7622TributylamineHCID 1670692-Chloro-1-methylpyridinium iodideHCID 674492293-ethyl-1-phenyl-1H-indazol-6-amine hydrochlorideHCID 178524171HCID 178524171、化合物

生成物 1

HCID 178437917HCID 178437917、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
100 °C

実験手順

Into a 100-mL 3-necked round-bottom flask, was placed a solution of 3-ethyl-1-phenyl-1H-indazol-6-amine hydrochloride (300 mg, 1.10 mmol, 1.00 equiv) in N,N-dimethylformamide (30 mL), tributylamine (492 mg, 2.66 mmol, 2.50 equiv), 1H-benzo[d]imidazole-5-carboxylic acid (180 mg, 1.11 mmol, 1.00 equiv), 2-chloro-1-methylpyridinium iodide (330 mg, 1.29 mmol, 1.20 equiv). The resulting solution was stirred for 2 days at 100° C. in an oil bath. The resulting mixture was concentrated under vacuum. The residue was applied onto a silica gel column with dichloromethane/methanol (50:1). The resulting mixture was diluted with methanol (10 mL) and the solids were washed with diethyl ether (1×50 mL) to yield N-(3-ethyl-1-phenyl-1H-indazol-6-yl)-1H-benzo[d]imidazole-5-carboxamide as a yellow solid.

後処理

  1. customInto a 100-mL 3-necked round-bottom flask, was placed
  2. concentrationThe resulting mixture was concentrated under vacuum
  3. additionThe resulting mixture was diluted with methanol (10 mL)
  4. washthe solids were washed with diethyl ether (1×50 mL)

出典と根拠

ORDレコード
ord-29a404dda10f4116845058069a887d7a
出典データセット
uspto-grants-2014_09
特許番号
US08822447B2

関連ノート

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