Lithium hydroxide, monohydrate → Lithium 5-chloro-2-(3-(4-(trifluoromethyl)phenoxy)pyrrolidin-1-yl)nicotinate

HRID 72485ノート

反応式

HRID 72485 の反応式
[Cl:1][C:2]1[CH:3]=[N:4][C:5]([N:12]2[CH2:16][CH2:15][CH:14]([O:17][C:18]3[CH:23]=[CH:22][C:21]([C:24]([F:27])([F:26])[F:25])=[CH:20][CH:19]=3)[CH2:13]2)=[C:6]([CH:11]=1)[C:7]([O:9]C)=[O:8].O.[OH-].[Li+:30]>O1CCOCC1.O>[Cl:1][C:2]1[CH:3]=[N:4][C:5]([N:12]2[CH2:16][CH2:15][CH:14]([O:17][C:18]3[CH:23]=[CH:22][C:21]([C:24]([F:25])([F:27])[F:26])=[CH:20][CH:19]=3)[CH2:13]2)=[C:6]([CH:11]=1)[C:7]([O-:9])=[O:8].[Li+:30]

参加物

4

反応物 2

HCID 168937Lithium hydroxide, monohydrateHCID 67958148Methyl 5-chloro-2-(3-(4-(trifluoromethyl)phenoxy)pyrrolidin-1-yl)nicotinate

生成物 1

HCID 67958430Lithium 5-chloro-2-(3-(4-(trifluoromethyl)phenoxy)pyrrolidin-1-yl)nicotinate収率 123.1%

試薬・触媒・溶媒 1

HCID 218864351,4-Dioxane--water (1/1)溶媒

反応条件

温度
150 °C

実験手順

To a mixture of methyl 5-chloro-2-(3-(4-(trifluoromethyl)phenoxy)pyrrolidin-1-yl)nicotinate (D91) (220 mg, 0.548 mmol) in a mixture 1,4-dioxane/water (2 ml/1 ml), lithium hydroxide monohydrate (34.55 mg, 0.823 mmol) was added and the resulting mixture was stirred at 150° C. under microwave irradiation for 10 min (2 cycles of 5 min each). Solvents were evaporated in vacuo to afford the title compound (D136) 265 mg

後処理

  1. additionwas added
  2. customSolvents were evaporated in vacuo

出典と根拠

ORDレコード
ord-93fdc44f85b94769ba8152fe08ebe39a
出典データセット
uspto-grants-2014_09
特許番号
US08828987B2

反応ノート

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