Sodium Hydroxide → (5-Chloro-2,3-dihydroindol-1-yl)-(6-chloropyrimidin-4-yl)-methanone

HRID 1640233

반응식

HRID 1640233 반응식
[Cl:1][C:2]1[N:7]=[CH:6][N:5]=[C:4]([C:8](Cl)=[O:9])[CH:3]=1.[Cl:11][C:12]1[CH:13]=[C:14]2[C:18](=[CH:19][CH:20]=1)[NH:17][CH2:16][CH2:15]2.[OH-].[Na+].C(=O)([O-])O.[Na+]>ClCCl>[Cl:11][C:12]1[CH:13]=[C:14]2[C:18](=[CH:19][CH:20]=1)[N:17]([C:8]([C:4]1[CH:3]=[C:2]([Cl:1])[N:7]=[CH:6][N:5]=1)=[O:9])[CH2:16][CH2:15]2

참가 물질

6

반응물 4

HCID 14798Sodium HydroxideHCID 1175965-ChloroindolineHCID 516892Sodium BicarbonateHCID 184220986-Chloropyrimidine-4-carbonyl chloride

생성물 1

HCID 58117515(5-Chloro-2,3-dihydroindol-1-yl)-(6-chloropyrimidin-4-yl)-methanone

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

1.5 g (8.48 mmol) 6-chloropyrimidine-4-carboxylic acid chloride in 50 mL dichloromethane were cooled with an ice/ethanol bath and combined with 1.2 g (7.81 mmol) 5-chloro-2,3-dihydro-1H-indole. 7.9 mL (7.9 mmol) of a 1M sodium hydroxide solution were added dropwise. The reaction mixture was stirred for 2 h with cooling and for 1 h at RT. The man 50 mL of an aqueous saturated sodium hydrogen carbonate solution were added. After 10 min stirring the organic phase was separated off and washed with water and 1 M hydrochloric acid. The organic phases was dried on magnesium sulphate, filtered and evaporated down i.vac.

후처리

  1. stirringAfter 10 min stirring the organic phase
  2. customwas separated off
  3. washwashed with water and 1 M hydrochloric acid
  4. customThe organic phases was dried on magnesium sulphate
  5. filtrationfiltered
  6. customevaporated down i.vac

출처 및 근거

ORD 기록
ord-9609d5247b264aa78617f25df36161f9
출처 데이터셋
uspto-grants-2012_02
특허 번호
US08110575B2

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