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

HRID 570544노트

반응식

HRID 570544 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-eddddf4136b64a6884bceb8be2a2c429
출처 데이터셋
uspto-grants-2015_05
특허 번호
US09023849B2

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