Hydrochloric Acid → HCID 86703895、化合物

HRID 471463

反応式

HRID 471463 の反応式
[CH2:1]([O:3][C:4]([C@H:6]1[CH2:8][C@@H:7]1[C:9]1[CH:14]=[CH:13][C:12]([O:15][C@H:16]2[C:24]3[C:19](=[C:20]([C:29]4[CH:34]=[CH:33][C:32]([OH:35])=[CH:31][CH:30]=4)[C:21]([C:25]([F:28])([F:27])[F:26])=[CH:22][CH:23]=3)[CH2:18][CH2:17]2)=[CH:11][CH:10]=1)=[O:5])[CH3:2].[O:36]1[C:38]2([CH2:43][CH2:42][O:41][CH2:40][CH2:39]2)[CH2:37]1.C(=O)([O-])[O-].[Cs+].[Cs+].Cl>CN(C)C=O.O>[CH2:1]([O:3][C:4]([C@H:6]1[CH2:8][C@@H:7]1[C:9]1[CH:10]=[CH:11][C:12]([O:15][C@H:16]2[C:24]3[C:19](=[C:20]([C:29]4[CH:34]=[CH:33][C:32]([O:35][CH2:37][C:38]5([OH:36])[CH2:43][CH2:42][O:41][CH2:40][CH2:39]5)=[CH:31][CH:30]=4)[C:21]([C:25]([F:26])([F:27])[F:28])=[CH:22][CH:23]=3)[CH2:18][CH2:17]2)=[CH:13][CH:14]=1)=[O:5])[CH3:2]

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 10796Cesium carbonateHCID 1604391,6-Dioxaspiro[2.5]octaneHCID 86703894HCID 86703894、化合物

生成物 1

HCID 86703895HCID 86703895、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

反応条件

温度
100 °C

実験手順

((1S,2S)-2-{4-[(R)-4-(4-Hydroxy-phenyl)-5-trifluoromethyl-indan-1-yloxy]-phenyl}-cyclopro-panecarboxylic acid ethyl ester (crude from step 2), 1,6-dioxa-spiro[2.5]octane (US2012/46304, 44 mg) and cesium carbonate (198 mg) are suspended in dry N,N-dimethylformamide and heated at 100° C. for 3 hours. The mixture is diluted with water, acidified with 0.2 M HCl solution and extracted with ethyl acetate. The combined organic extracts are concentrated under vacuum and the residue purified by flash chromatography (0-30% EtOAc in cyclohexane) ti give the title compound (yield 50 mg).

後処理

  1. extractionextracted with ethyl acetate
  2. concentrationThe combined organic extracts are concentrated under vacuum
  3. customthe residue purified by flash chromatography (0-30% EtOAc in cyclohexane) ti

出典と根拠

ORDレコード
ord-2ef9da7c07234a1bbac33a7b94f0ad9d
出典データセット
uspto-grants-2014_01
特許番号
US08633182B2

関連ノート

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