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Water → 6-chloro-N5-(2,2-difluoroethyl)-1-ethyl-N2-{2,2,2-trifluoro-1-[4-fluoro-3-(trifluoromethyl)phenyl]ethyl}-1H-indole-2,5-dicarboxamide

HRID 514246
ノート
印刷プレビュー

反応式

HRID 514246 の反応式
[F:1][CH:2]([F:5])[CH2:3][NH2:4].C[Al](C)C.ClC1[CH:19]=[C:18]2[C:14]([CH:15]=[C:16]([C:22](=[O:40])[NH:23][CH:24]([C:29]3[CH:34]=[CH:33][C:32]([F:35])=[C:31]([C:36]([F:39])([F:38])[F:37])[CH:30]=3)[C:25]([F:28])([F:27])[F:26])[N:17]2[CH2:20][CH3:21])=[CH:13][C:12]=1[C:41]([O:43]CC)=O.O.Cl[CH2:48][Cl:49]>>[Cl:49][C:48]1[CH:19]=[C:18]2[C:14]([CH:15]=[C:16]([C:22]([NH:23][CH:24]([C:29]3[CH:34]=[CH:33][C:32]([F:35])=[C:31]([C:36]([F:37])([F:38])[F:39])[CH:30]=3)[C:25]([F:28])([F:26])[F:27])=[O:40])[N:17]2[CH2:20][CH3:21])=[CH:13][C:12]=1[C:41]([NH:4][CH2:3][CH:2]([F:5])[F:1])=[O:43]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 5

HCID 962WaterHCID 6344Dichloromethane3 回HCID 1362742,2-DifluoroethanamineHCID 16682925TrimethylaluminumHCID 86713970ethyl 6-chloro-1-ethyl-2-({2,2,2-trifluoro-1-[4-fluoro-3-(trifluoromethyl)phenyl]ethyl}carbamoyl)-1H-indole-5-carboxylate

生成物 1

HCID 86713971
6-chloro-N5-(2,2-difluoroethyl)-1-ethyl-N2-{2,2,2-trifluoro-1-[4-fluoro-3-(trifluoromethyl)phenyl]ethyl}-1H-indole-2,5-dicarboxamide
収率 81%

実験手順

2,2-Difluoroethanamine (0.12 g, 1.42 mmol) was dissolved under argon in dichloromethane (2 ml). At room temperature, a solution of trimethylaluminium in dichloromethane (0.71 ml, 1.42 mmol) was added dropwise. The reaction mixture was stirred at room temperature for 30 min and then a solution of ethyl 6-chloro-1-ethyl-2-({2,2,2-trifluoro-1-[4-fluoro-3-(trifluoromethyl)phenyl]ethyl}carbamoyl)-1H-indole-5-carboxylate (0.078 g, 0.14 mmol) in dichloromethane (2 ml) was added dropwise. The reaction mixture was heated under reflux for 16 h and, after cooling, water was added. The aqueous phase was extracted three times with ethyl acetate. The combined organic phases were dried over sodium sulphate and the solvent was removed under reduced pressure. The residue was chromatographed with cyclohexane/ethyl acetate (4/1) and gave 0.065 g (81% of theory) of 6-chloro-N5-(2,2-difluoroethyl)-1-ethyl-N2-{2,2,2-trifluoro-1-[4-fluoro-3-(trifluoromethyl)phenyl]ethyl}-1H-indole-2,5-dicarboxamide.

後処理

  1. temperatureThe reaction mixture was heated
  2. temperatureunder reflux for 16 h
  3. temperatureafter cooling
  4. extractionThe aqueous phase was extracted three times with ethyl acetate
  5. dry with materialThe combined organic phases were dried over sodium sulphate
  6. customthe solvent was removed under reduced pressure
  7. customThe residue was chromatographed with cyclohexane/ethyl acetate (4/1)

出典と根拠

ORDレコード
ord-d36805a538d3439096a2867929ae4c45
出典データセット
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09107411B2

反応ノート

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