Sodium Methoxide → HCID 20483476, 화합물

HRID 1701741노트

반응식

HRID 1701741 반응식
[Cl:1][C:2]1[C:3]([O:8][CH2:9][CH:10]([OH:16])[CH2:11][NH:12][CH:13]([CH3:15])[CH3:14])=[N:4][CH:5]=[CH:6][N:7]=1.[CH3:17][O-:18].[Na+]>CO>[ClH:1].[CH3:17][O:18][C:2]1[C:3]([O:8][CH2:9][CH:10]([OH:16])[CH2:11][NH:12][CH:13]([CH3:15])[CH3:14])=[N:4][CH:5]=[CH:6][N:7]=1

참가 물질

4

반응물 2

HCID 10942334Sodium MethoxideHCID 204834181-[(3-Chloropyrazin-2-yl)oxy]-3-[(propan-2-yl)amino]propan-2-ol

생성물 1

HCID 20483476HCID 20483476, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

7.5 g of 3-chloro-2-(3'-isopropylamino-2'-hydroxy-propoxy)-pyrazine and 3.2 g of sodium methylate in 150 ml of methanol are boiled for 10 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 acid aqueous 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 crude base is thus obtained, from which 3-methoxy-2-(3'-isopropylamino-2'-hydroxy-propoxy)-pyrazine hydrochloride, melting point 152°-153° C., is obtained by reaction with ethereal hydrochloric acid in methanol.

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

출처 및 근거

ORD 기록
ord-ee198cdb44454aa3a32b3279f8c0b005
출처 데이터셋
uspto-grants-1980_03
특허 번호
US04195090

반응 노트

불러오는 중…