Isopropylamine → 1-[(3-Chloropyrazin-2-yl)oxy]-3-[(propan-2-yl)amino]propan-2-ol

HRID 647963노트

반응식

HRID 647963 반응식
Br[CH2:2][CH:3]([OH:13])[CH2:4][O:5][C:6]1[C:11]([Cl:12])=[N:10][CH:9]=[CH:8][N:7]=1.[CH:14]([NH2:17])([CH3:16])[CH3:15]>CO>[Cl:12][C:11]1[C:6]([O:5][CH2:4][CH:3]([OH:13])[CH2:2][NH:17][CH:14]([CH3:16])[CH3:15])=[N:7][CH:8]=[CH:9][N:10]=1

참가 물질

4

실험 절차

53 g of 2-(3'-bromo-2'-hydroxy-propoxy)-3-chloropyrazine and 59 g of isopropylamine in 500 ml of methanol are boiled for 15 hours under reflux. The reaction mixture is then evaporated in a waterpump vacuum. The residue is partitioned between 2 N hydrochloric acid and ether. The hydrochloric acid phase is rendered alkaline with concentrated sodium hydroxide solution and extracted by shaking with ether. The ether extracts are washed with water, dried over sodium sulphate and evaporated in a waterpump vacuum. The residue crystallises from ether. 3-Chloro-2-(3'-isopropylamino-2'-hydroxy-propoxy)-pyrazine, melting point 99°-100° C., is thus obtained.

후처리

  1. temperatureunder reflux
  2. customThe reaction mixture is then evaporated in a waterpump vacuum
  3. customThe residue is partitioned between 2 N hydrochloric acid and ether
  4. extractionextracted
  5. washThe ether extracts are washed with water
  6. dry with materialdried over sodium sulphate
  7. customevaporated in a waterpump vacuum
  8. customThe residue crystallises from ether

출처 및 근거

ORD 기록
ord-2974a0b5f33a469b90345df39891c274
출처 데이터셋
uspto-grants-1983_10
특허 번호
US04410530

반응 노트

불러오는 중…