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Sodium Hydroxide → HCID 58117525、化合物

HRID 1640239
ノート
印刷プレビュー

反応式

HRID 1640239 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

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

生成物 1

HCID 58117525HCID 58117525、化合物

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒
HCID 6344
Dichloromethane
溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-d02bba889ed445658dd40c147aec7aad
出典データセット
uspto-grants-2012_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08110575B2

反応ノート

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