Trifluoroacetic acid → HCID 178502740, 화합물

HRID 271349노트

반응식

HRID 271349 반응식
C([O:5][C:6](=[O:18])[CH2:7][C@H:8]1[CH2:11][C@@H:10]([C:12](=[O:17])[N:13]([O:15][CH3:16])[CH3:14])[CH2:9]1)(C)(C)C.FC(F)(F)C(O)=O>ClCCl>[CH3:16][O:15][N:13]([CH3:14])[C:12]([C@@H:10]1[CH2:11][C@H:8]([CH2:7][C:6]([OH:18])=[O:5])[CH2:9]1)=[O:17]

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 178502741HCID 178502741, 화합물

생성물 1

HCID 178502740HCID 178502740, 화합물수율 102.3%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To an ice cold solution of 2 g of cis-[3-(methoxy-methyl-carbamoyl)-cyclobutyl]-acetic acid tert-butyl ester in 25 mL of dichloromethane was added 10 mL of trifluoroacetic acid. The mixture was allowed to warm and stir for 2 h then concentrated under reduced pressure. The residue was taken up in 3×50 mL of toluene and repeatedly concentrated under reduced pressure to remove trifluoroacetic acid. Drying under vacuum overnight gave 1.6 g of product as a colorless oil: MS (m+1)=202.3; 1H NMR (400 MHz, CDCl3) 9.0 (br s, 1H), 3.62 (s, 3H), 3.18 (s, 3H), 2.65 (m, 1H), 2.5 (overlapping d and m, 3H), 2.4 (dd, 1H), 2.0 (, m, 2H).

후처리

  1. temperatureto warm
  2. concentrationthen concentrated under reduced pressure
  3. concentrationrepeatedly concentrated under reduced pressure
  4. customto remove trifluoroacetic acid
  5. customDrying under vacuum overnight

출처 및 근거

ORD 기록
ord-860d91fe54e443459ff03a0de0adcc89
출처 데이터셋
uspto-grants-2008_11
특허 번호
US07452893B2

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