2-(Trifluoromethyl)aniline → HCID 68973195、化合物

HRID 749049ノート

反応式

HRID 749049 の反応式
CN1CCOCC1.[F:8][C:9]([F:18])([F:17])[C:10]1[CH:16]=[CH:15][CH:14]=[CH:13][C:11]=1[NH2:12].[O:19]=[C:20]1[CH2:37][CH2:36][C@@:35]2([CH3:38])[C:22]([CH2:23][CH2:24][C@@H:25]3[C@@H:34]2[CH2:33][CH2:32][C@@:30]2([CH3:31])[C@H:26]3[CH2:27][CH2:28][C@@H:29]2[C:39](Cl)=[O:40])=[CH:21]1>C(Cl)Cl>[O:19]=[C:20]1[CH2:37][CH2:36][C@@:35]2([CH3:38])[C:22]([CH2:23][CH2:24][C@@H:25]3[C@@H:34]2[CH2:33][CH2:32][C@@:30]2([CH3:31])[C@H:26]3[CH2:27][CH2:28][C@@H:29]2[C:39]([NH:12][C:11]2[CH:13]=[CH:14][CH:15]=[CH:16][C:10]=2[C:9]([F:17])([F:18])[F:8])=[O:40])=[CH:21]1

参加物

5

反応物 3

HCID 69222-(Trifluoromethyl)anilineHCID 79724-MethylmorpholineHCID 117273863-Oxoandrost-4-ene-17beta-carbonyl chloride

生成物 1

HCID 68973195HCID 68973195、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To a solution of N-methylmorpholine (0.28 g, 2.8 mmol) and 2-(trifluoromethyl)aniline (0.5 g, 3.1 mmol) in anhydrous CH2Cl2 (3.0 mL) at 0° C. under a nitrogen atmosphere was added a solution of 3-oxoandrost-4-ene-17β-carbonyl chloride from Step A (2.56 mmol) in anhydrous CH2Cl2 (8.1 mL) dropwise. The ice bath was removed and the mixture stirred at room temperature overnight. The reaction was then concentrated and the residue was purified by flash chromatography on silica gel eluting with 0 to 50% EtOAc-hexanes to afford the desired product as a white solid.

後処理

  1. customThe ice bath was removed
  2. concentrationThe reaction was then concentrated
  3. customthe residue was purified by flash chromatography on silica gel eluting with 0 to 50% EtOAc-hexanes

出典と根拠

ORDレコード
ord-ac4f7277ab204c88874899af40acec3c
出典データセット
uspto-grants-2008_07
特許番号
US07402577B2

反応ノート

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