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Trifluoroacetic acid → rac-(2'S,3'R,4'S,5'R)-6-chloro-4'-(3-chloro-2-fluoro-phenyl)-2'-(2,2-dimethyl-propyl)-2-oxo-1,2-dihydro-spiro[indole-3,3'-pyrrolidine]-5'-carboxylic acid (1-methyl-1H-pyrrol-2-yl)-amide

HRID 417353
ノート
印刷プレビュー

反応式

HRID 417353 の反応式
C(OC([C:8]1[N:9]([CH3:44])[C:10]([NH:13][C:14]([C@@H:16]2[NH:20][C@@H:19]([CH2:21][C:22]([CH3:25])([CH3:24])[CH3:23])[C@:18]3([C:33]4[C:28](=[CH:29][C:30]([Cl:34])=[CH:31][CH:32]=4)[NH:27][C:26]3=[O:35])[C@H:17]2[C:36]2[CH:41]=[CH:40][CH:39]=[C:38]([Cl:42])[C:37]=2[F:43])=[O:15])=[CH:11][CH:12]=1)=O)(C)(C)C.FC(F)(F)C(O)=O>ClCCl>[CH3:44][N:9]1[CH:8]=[CH:12][CH:11]=[C:10]1[NH:13][C:14]([CH:16]1[NH:20][CH:19]([CH2:21][C:22]([CH3:25])([CH3:24])[CH3:23])[C:18]2([C:33]3[C:28](=[CH:29][C:30]([Cl:34])=[CH:31][CH:32]=3)[NH:27][C:26]2=[O:35])[CH:17]1[C:36]1[CH:41]=[CH:40][CH:39]=[C:38]([Cl:42])[C:37]=1[F:43])=[O:15]
参加物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 6422Trifluoroacetic acidHCID 58286361HCID 58286361、化合物

生成物 1

HCID 76741112rac-(2'S,3'R,4'S,5'R)-6-chloro-4'-(3-chloro-2-fluoro-phenyl)-2'-(2,2-dimethyl-propyl)-2-oxo-1,2-dihydro-spiro[indole-3,3'-pyrrolidine]-5'-carboxylic acid (1-methyl-1H-pyrrol-2-yl)-amide収率 109.3%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A solution of rac-5-{[(2′S,3′R,4′S,5′R)-6-chloro-4′-(3-chloro-2-fluoro-phenyl)-2′-(2,2-dimethyl-propyl)-2-oxo-1,2-dihydro-spiro[indole-3,3′-pyrrolidine]-5′-carbonyl]amino}-1-methyl-1H-pyrrole-2-carboxylic acid tert-butyl ester (0.1 g, 0.16 mmol) in dichloromethane (2 mL) was added trifluoroacetic acid (2 mL). The reaction mixture was stirred at room temperature for 20 h, then concentrated. To the residue was added aqueous saturated NaHCO3 solution until “pH” became 7-8, and the mixture was extracted with ethyl acetate several times. The combined organic extract was washed with water, brine, dried over MgSO4, and concentrated to give rac-(2′S,3′R,4′S,5′R)-6-chloro-4′-(3-chloro-2-fluoro-phenyl)-2′-(2,2-dimethyl-propyl)-2-oxo-1,2-dihydro-spiro[indole-3,3′-pyrrolidine]-5′-carboxylic acid (1-methyl-1H-pyrrol-2-yl)-amide as a light brown solid (95 mg, 93%).

後処理

  1. concentrationconcentrated
  2. additionTo the residue was added aqueous saturated NaHCO3 solution until “pH”
  3. extractionthe mixture was extracted with ethyl acetate several times
  4. extractionThe combined organic extract
  5. washwas washed with water, brine
  6. dry with materialdried over MgSO4
  7. concentrationconcentrated

出典と根拠

ORDレコード
ord-404fa4246d45443685ebcc94d69d226c
出典データセット
uspto-grants-2012_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08088815B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート