Trifluoroacetic acid → 3-(3-Chloro-5-fluorophenyl)-3-methoxypyrrolidine

HRID 1188197노트

반응식

HRID 1188197 반응식
C(OC([N:8]1[CH2:12][CH2:11][C:10]([C:15]2[CH:20]=[C:19]([F:21])[CH:18]=[C:17]([Cl:22])[CH:16]=2)([O:13][CH3:14])[CH2:9]1)=O)(C)(C)C.FC(F)(F)C(O)=O>C(Cl)Cl>[Cl:22][C:17]1[CH:16]=[C:15]([C:10]2([O:13][CH3:14])[CH2:11][CH2:12][NH:8][CH2:9]2)[CH:20]=[C:19]([F:21])[CH:18]=1

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 67402360Tert-butyl 3-(3-chloro-5-fluorophenyl)-3-methoxypyrrolidin-1-carboxylate

생성물 1

HCID 462192233-(3-Chloro-5-fluorophenyl)-3-methoxypyrrolidine수율 77.1%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of tert-butyl-3-(3-chloro-5-fluorophenyl)-3-methoxypyrrolidin-1-carboxylate (1.57 g, 4.77 mmol) in methylene chloride (20 mL), was added trifluoroacetic acid (5 mL). The mixture was stirred for 1 h at ambient temperature after which the solvent was evaporated. Purification on a Biotage Isolute SCX-3 SPE column (washed with methanol and eluted with methanol/triethylamine, 4:1) gave the title compound (0.845 g, 77%). MS m/z (rel. intensity, 70 eV) 199 (bp), 187 (93), 157 (61), 133 (66), 129 (59).

후처리

  1. customwas evaporated
  2. customPurification
  3. washon a Biotage Isolute SCX-3 SPE column (washed with methanol and eluted with methanol/triethylamine, 4:1)

출처 및 근거

ORD 기록
ord-5169c72abb284707b3633f91cf378bd4
출처 데이터셋
uspto-grants-2014_03
특허 번호
US08673962B2

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