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Trifluoroacetic acid → 4-(4-Amino-3-chloro-5-trifluoromethyl-phenyl)-3,3-bis-ethoxycarbonyl-butanoic acid

HRID 494752
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HRID 494752 반응식
[NH2:1][C:2]1[C:7]([C:8]([F:11])([F:10])[F:9])=[CH:6][C:5]([CH2:12][C:13]([C:27]([O:29][CH2:30][CH3:31])=[O:28])([C:22]([O:24][CH2:25][CH3:26])=[O:23])[CH2:14][C:15]([O:17]C(C)(C)C)=[O:16])=[CH:4][C:3]=1[Cl:32].C(O)(C(F)(F)F)=O>C(Cl)Cl>[NH2:1][C:2]1[C:7]([C:8]([F:9])([F:10])[F:11])=[CH:6][C:5]([CH2:12][C:13]([C:22]([O:24][CH2:25][CH3:26])=[O:23])([C:27]([O:29][CH2:30][CH3:31])=[O:28])[CH2:14][C:15]([OH:17])=[O:16])=[CH:4][C:3]=1[Cl:32]
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참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 68590557Tert. butyl 4-(4-amino-3-chloro-5-trifluoromethyl-phenyl)-3,3-bis-ethoxycarbonyl-butyrate2회

생성물 1

HCID 221846134-(4-Amino-3-chloro-5-trifluoromethyl-phenyl)-3,3-bis-ethoxycarbonyl-butanoic acid

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 30.0 g (62.25 mmol) tert. butyl 4-(4-amino-3-chloro-5-trifluoromethyl-phenyl)-3,3-bis-ethoxycarbonyl-butyrate (Intermediate product 65) in 200 mL CH2Cl2 was added 20 mL TFA while cooling with ice and the mixture was stirred for 16 hours at RT. The reaction mixture was evaporated i. vac. and the residue recrystallised from petroleum ether. The precipitate was filtered off, washed with petroleum ether and dried.

후처리

  1. temperaturewhile cooling with ice
  2. customThe reaction mixture was evaporated i
  3. customand the residue recrystallised from petroleum ether
  4. filtrationThe precipitate was filtered off
  5. washwashed with petroleum ether
  6. customdried

출처 및 근거

ORD 기록
ord-bea2455ae5c8407e9ce1bdd836c3241d
출처 데이터셋
uspto-grants-2009_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07538115B2

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