Triethylamine → 4-Butyloxazolidine-2-thione

HRID 1721285

반응식

HRID 1721285 반응식
[CH3:1][CH2:2][CH2:3][CH2:4][CH:5]([NH2:8])[CH2:6][OH:7].C(N(CC)CC)C.[C:16](Cl)(Cl)=[S:17]>C1COCC1>[CH2:4]([CH:5]1[CH2:6][O:7][C:16](=[S:17])[NH:8]1)[CH2:3][CH2:2][CH3:1]

참가 물질

5

반응 조건

온도
20 °C

실험 절차

To a stirred cold solution of DL-2-amino-1-hexanol (1.1 ml) in dry THF (10 ml) was added triethylamine (2.8 ml) followed by dropwise addition of thiophosgene (0.81 ml) in dry THF (9 ml). The mixture was then stirred for 18 h at 20° C., evaporated under reduced pressure and the residue partitioned between water and diethylether. The ether extract was dried with sodium sulphate filtered and evaporated. The residue was dissolved in the minimum of hot 1:1 dimethylether-hexane and crystallised on cooling to give 4-butyloxazolidine-2-thione, mp 71°-2°.

후처리

  1. customevaporated under reduced pressure
  2. customthe residue partitioned between water and diethylether
  3. extractionThe ether extract
  4. dry with materialwas dried with sodium sulphate
  5. filtrationfiltered
  6. customevaporated
  7. dissolutionThe residue was dissolved in the minimum of hot 1:1 dimethylether-hexane
  8. customcrystallised
  9. temperatureon cooling

출처 및 근거

ORD 기록
ord-3635554a77c149f9b9b46b6e1e667db9
출처 데이터셋
uspto-grants-1996_04
특허 번호
US05510344

연결된 노트

불러오는 중…