Sodium Hydroxide → 3-(3-(Pyrimidin-4-yl)pyridin-2-ylamino)-4-(trifluoromethyl)benzoic acid

HRID 446315ノート

反応式

HRID 446315 の反応式
[N:1]1[CH:6]=[CH:5][C:4]([C:7]2[C:8]([NH:13][C:14]3[CH:15]=[C:16]([CH:22]=[CH:23][C:24]=3[C:25]([F:28])([F:27])[F:26])[C:17]([O:19]CC)=[O:18])=[N:9][CH:10]=[CH:11][CH:12]=2)=[N:3][CH:2]=1.[OH-].[Na+]>CCO>[N:1]1[CH:6]=[CH:5][C:4]([C:7]2[C:8]([NH:13][C:14]3[CH:15]=[C:16]([CH:22]=[CH:23][C:24]=3[C:25]([F:28])([F:26])[F:27])[C:17]([OH:19])=[O:18])=[N:9][CH:10]=[CH:11][CH:12]=2)=[N:3][CH:2]=1

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 66970285Ethyl 3-(3-(pyrimidin-4-yl)pyridin-2-ylamino)-4-(trifluoromethyl)benzoate

生成物 1

HCID 669704063-(3-(Pyrimidin-4-yl)pyridin-2-ylamino)-4-(trifluoromethyl)benzoic acid

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

Ethyl 3-(3-(pyrimidin-4-yl)pyridin-2-ylamino)-4-(trifluoromethyl)benzoate (2.50 g, 6 mmol) was suspended in EtOH (30 ml) and treated with 5N Sodium hydroxide (4 ml). The mixture was stirred at reflux overnight. The reaction was cooled down and the volatiles removed in vacuo. The residue was washed with diluted acetic acid (10:1 water:acetic acid) and then washed with water, to give 3-(3-(pyrimidin-4-yl)pyridin-2-ylamino)-4-(trifluoromethyl)benzoic acid as a yellow solid, after drying in a vacuum oven at 60° C. overnight. MS m/z=361 [M+1]+. Calc'd for C17H11F3N4O2: 360.08.

後処理

  1. temperatureat reflux overnight
  2. temperatureThe reaction was cooled down
  3. customthe volatiles removed in vacuo
  4. washThe residue was washed with diluted acetic acid (10:1 water:acetic acid)
  5. washwashed with water

出典と根拠

ORDレコード
ord-6136ae04b633421cb718b07fe11948d9
出典データセット
uspto-grants-2013_07
特許番号
US08476434B2

反応ノート

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