Methanol → HCID 66673635, 화합물

HRID 870270노트

반응식

HRID 870270 반응식
[CH3:1][O:2][C:3](=[O:16])[C@@H:4]([CH2:9][CH:10]1[CH2:15][CH2:14][CH2:13][CH2:12][CH2:11]1)[CH2:5][C:6](O)=[O:7].B.CO>O1CCCC1>[CH3:1][O:2][C:3](=[O:16])[C@@H:4]([CH2:9][CH:10]1[CH2:11][CH2:12][CH2:13][CH2:14][CH2:15]1)[CH2:5][CH2:6][OH:7]

참가 물질

5

실험 절차

A mixture of (S)-2-cyclohexylmethyl-succinic acid 1-methyl ester (60.0 g, 263 mmol) and tetrahydrofuran (600 mL) was stirred at room temperature and then cooled to −5° C. over 30 min. To the reaction mixture was added 1.0 M borane in tetrahydrofuran (520 mL) dropwise over 45 min, keeping the internal temperature below 0° C. To the reaction mixture was added MeOH (100 mL) dropwise to quench the reaction. The reaction mixture was concentrated to about 100 mL by rotary evaporation. (Trifluoromethyl)benzene (200 mL) was added and volume was reduced to 25 mL by rotary evaporation. (Trifluoromethyl)benzene (100 mL) was added to the resulting thick oil and the volume was reduced to ˜25 mL to provide crude title product (56.3 g).

후처리

  1. temperaturecooled to −5° C. over 30 min
  2. customthe internal temperature below 0° C
  3. customto quench
  4. customthe reaction
  5. concentrationThe reaction mixture was concentrated to about 100 mL by rotary evaporation
  6. addition(Trifluoromethyl)benzene (200 mL) was added
  7. customvolume was reduced to 25 mL by rotary evaporation
  8. addition(Trifluoromethyl)benzene (100 mL) was added to the resulting thick oil

출처 및 근거

ORD 기록
ord-87b8b791e23c46979899c4225f88986d
출처 데이터셋
uspto-grants-2015_03
특허 번호
US08969370B2

반응 노트

불러오는 중…