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Sodium Hydroxide → HCID 58117525, 화합물

HRID 1640239
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HRID 1640239 반응식
[CH2:1]([NH:9][CH2:10][C:11]([F:14])([F:13])[F:12])[CH2:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.[OH-].[Na+].[Cl:17][C:18]1[N:23]=[CH:22][N:21]=[C:20]([C:24](Cl)=[O:25])[CH:19]=1.C(=O)([O-])O.[Na+]>ClCCl.C(O)C>[Cl:17][C:18]1[N:23]=[CH:22][N:21]=[C:20]([C:24]([N:9]([CH2:1][CH2:2][C:3]2[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=2)[CH2:10][C:11]([F:12])([F:13])[F:14])=[O:25])[CH:19]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 14798Sodium HydroxideHCID 516892Sodium BicarbonateHCID 135556072,2,2-Trifluoro-N-(2-phenylethyl)ethan-1-amineHCID 184220986-Chloropyrimidine-4-carbonyl chloride

생성물 1

HCID 58117525HCID 58117525, 화합물

시약·촉매·용매 2

HCID 702Ethanol용매
HCID 6344
Dichloromethane
용매

실험 절차

0.80 g (3.94 mmol) phenethyl-(2,2,2-trifluoroethyl)-amine and 3.9 mL (3.9 mmol) of a 1M sodium hydroxide solution were added dropwise to 0.77 g (4.33 mmol) 6-chloropyrimidine-4-carboxylic acid chloride in 20 mL dichloromethane while cooling with a bath of ice and ethanol. The mixture was first stirred for 2 h with cooling and then for 1 h at RT. 50 mL of a saturated sodium hydrogen carbonate solution were added and the mixture was stirred for 10 min. The organic phase was separated off, washed with water and 1M hydrochloric acid, dried on sodium sulphate, filtered and concentrated by rotary evaporation i.vac.

후처리

  1. temperaturewith cooling
  2. waitfor 1 h at RT
  3. stirringthe mixture was stirred for 10 min
  4. customThe organic phase was separated off
  5. washwashed with water and 1M hydrochloric acid
  6. customdried on sodium sulphate
  7. filtrationfiltered
  8. concentrationconcentrated by rotary evaporation i.vac

출처 및 근거

ORD 기록
ord-d02bba889ed445658dd40c147aec7aad
출처 데이터셋
uspto-grants-2012_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08110575B2

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