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2-Chloro-5-(trifluoromethyl)benzoyl chloride → Ethyl 4-(2-chloro-5-(trifluoromethyl)benzamido)-2-methylcyclohexane carboxylate

HRID 1914638
ノート
印刷プレビュー

反応式

HRID 1914638 の反応式
[NH2:1][CH:2]1[CH2:7][CH2:6][CH:5]([C:8]([O:10][CH2:11][CH3:12])=[O:9])[CH:4]([CH3:13])[CH2:3]1.[Cl:14][C:15]1[CH:23]=[CH:22][C:21]([C:24]([F:27])([F:26])[F:25])=[CH:20][C:16]=1[C:17](Cl)=[O:18]>C1COCC1>[Cl:14][C:15]1[CH:23]=[CH:22][C:21]([C:24]([F:25])([F:26])[F:27])=[CH:20][C:16]=1[C:17]([NH:1][CH:2]1[CH2:7][CH2:6][CH:5]([C:8]([O:10][CH2:11][CH3:12])=[O:9])[CH:4]([CH3:13])[CH2:3]1)=[O:18]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 27781062-Chloro-5-(trifluoromethyl)benzoyl chlorideHCID 57465891Ethyl 4-amino-2-methylcyclohexane-1-carboxylate

生成物 1

HCID 57465893Ethyl 4-(2-chloro-5-(trifluoromethyl)benzamido)-2-methylcyclohexane carboxylate

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
0 °C

実験手順

Ethyl 4-amino-2-methylcyclohexanecarboxylate (780 mg, 4.21 mmol) in THF (10 ml) is treated with TEA (1.174 ml, 8.42 mmol) and the reaction mixture is cooled to 0° C. 2-Chloro-5-(trifluoromethyl)benzoyl chloride (921 mg, 3.79 mmol) is added dropwise and the reaction mixture is stirred and allowed to warm to RT. After 3 hours, the reaction is quenched with water and partitioned between EtOAc and sat. sodium bicarbonate. The organic portion is separated and dried over MgSO4 and concentrated in vacuo to afford the title compound which is used without further purification. [MH]+392.26.

後処理

  1. temperatureto warm to RT
  2. customthe reaction is quenched with water
  3. custompartitioned between EtOAc and sat. sodium bicarbonate
  4. customThe organic portion is separated
  5. dry with materialdried over MgSO4
  6. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-70adbd8794814d348469f2dffe36bccb
出典データセット
uspto-grants-2013_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08614213B2

反応ノート

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