Water → 6-Chloro-1-(2-fluorobenzyl)-1H-indazole-3-carbonitrile

HRID 570544ノート

反応式

HRID 570544 の反応式
[F:1][C:2]1[CH:9]=[CH:8][CH:7]=[CH:6][C:3]=1[CH2:4]Br.[Cl:10][C:11]1[CH:19]=[C:18]2[C:14]([C:15]([C:20]#[N:21])=[N:16][NH:17]2)=[CH:13][CH:12]=1.C(=O)([O-])[O-].[K+].[K+].O>CN(C=O)C>[Cl:10][C:11]1[CH:19]=[C:18]2[C:14]([C:15]([C:20]#[N:21])=[N:16][N:17]2[CH2:4][C:3]2[CH:6]=[CH:7][CH:8]=[CH:9][C:2]=2[F:1])=[CH:13][CH:12]=1

参加物

6

反応物 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 67968alpha-Bromo-o-fluorotolueneHCID 534084026-Chloro-1H-indazole-3-carbonitrile

生成物 1

HCID 866921116-Chloro-1-(2-fluorobenzyl)-1H-indazole-3-carbonitrile収率 102.3%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

実験手順

Under argon, 2.45 ml (14.2 mmol) of 2-fluorobenzyl bromide, dissolved in 10 ml DMF, were added to a mixture of 2.3 g (12.9 mmol) of 6-chloro-1H-indazole-3-carbonitrile (WO 2011/149921, Expl. 58C) and 2.15 g (15.5 mmol) of potassium carbonate in 40 ml of DMF, and the mixture was stirred at RT overnight. Then the mixture was poured onto 90 ml of water and the mixture was stirred at room temperature for 30 min. The precipitated solids were filtered off, washed with water and dried under high vacuum overnight. 3.77 g of the title compound were obtained as a crude product.

後処理

  1. stirringthe mixture was stirred at room temperature for 30 min
  2. filtrationThe precipitated solids were filtered off
  3. washwashed with water
  4. customdried under high vacuum overnight

出典と根拠

ORDレコード
ord-eddddf4136b64a6884bceb8be2a2c429
出典データセット
uspto-grants-2015_05
特許番号
US09023849B2

反応ノート

読み込み中…