Dichloromethane → (1R,2R)-2-tert-butyldiphenylsilanyloxy-1-(3,4,5-trifluorophenyl)propylamine

HRID 16358

反応式

HRID 16358 の反応式
FC(F)(F)C(O)=O.C(Cl)Cl.C(OC(=O)[NH:17][C@H:18]([C:39]1[CH:44]=[C:43]([F:45])[C:42]([F:46])=[C:41]([F:47])[CH:40]=1)[C@H:19]([O:21][Si:22]([C:35]([CH3:38])([CH3:37])[CH3:36])([C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1)[C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1)[CH3:20])(C)(C)C.C(=O)([O-])O.[Na+]>C(OCC)(=O)C>[Si:22]([O:21][C@H:19]([CH3:20])[C@H:18]([NH2:17])[C:39]1[CH:44]=[C:43]([F:45])[C:42]([F:46])=[C:41]([F:47])[CH:40]=1)([C:35]([CH3:36])([CH3:37])[CH3:38])([C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1)[C:23]1[CH:24]=[CH:25][CH:26]=[CH:27][CH:28]=1

参加物

6

実験手順

Trifluoroacetic acid (0.5 mL) was added to a methylene chloride solution (2 mL) of [(1R,2R)-2-tert-butyldiphenylsilanyloxy-1-(3,4,5-trifluorophenyl)propyl]carbamic acid tert-butyl ester (370 mg). The resulting reaction solution was stirred at room temperature for 11 hr, and a saturated sodium hydrogencarbonate aqueous solution and ethyl acetate were added thereto. The organic layer was separated, washed with a saturated sodium hydrogencarbonate aqueous solution and with saturated saline in this order, and concentrated under reduced pressure to give 275 mg of the title compound. The physical property values of this compound were as follows:

後処理

  1. customThe resulting reaction solution
  2. customThe organic layer was separated
  3. washwashed with a saturated sodium hydrogencarbonate aqueous solution and with saturated saline in this order
  4. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-d1b2a85d4dcb4ddd8eee5a9a2e019bbc
出典データセット
uspto-grants-2010_06
特許番号
US07737141B2

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