3-bromo-11H-s-triazolo[3,4-b][3]benzazepine → 3-methoxy-11H-s-triazolo[3,4-b][3]benzazepine

HRID 26526노트

반응식

HRID 26526 반응식
Br[C:2]1[N:11]2[C:5]([CH2:6][C:7]3[CH:15]=[CH:14][CH:13]=[CH:12][C:8]=3[CH:9]=[CH:10]2)=[N:4][N:3]=1.[CH3:16][O-:17].[Na+].CO>CO>[CH3:16][O:17][C:2]1[N:11]2[C:5]([CH2:6][C:7]3[CH:15]=[CH:14][CH:13]=[CH:12][C:8]=3[CH:9]=[CH:10]2)=[N:4][N:3]=1

참가 물질

4

반응물 2

HCID 213233903-bromo-11H-s-triazolo[3,4-b][3]benzazepineHCID 23694274Sodium methanolate methanol

생성물 1

HCID 213233683-methoxy-11H-s-triazolo[3,4-b][3]benzazepine

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a solution of 0.262 g of 3-bromo-11H-s-triazolo [3,4-b][3]benzazepine in 2 ml of methanol was added 1.0 ml of 2 N-sodium methoxide/methanol and the mixture was refluxed for one hour. The solvent was evaporated off and, following the addition of water, the residue was extracted with ethyl acetate. The ethyl acetate layer was washed with water and dried over Na2SO4. The solvent was then evaporated off and the residue was treated with isopropyl ether. By the above procedure was obtained 3-methoxy-11H-s-triazolo[3,4-b][3]benzazepine as crystals. Recrystallization from ethyl acetate-n-hexane yielded colorless prisms, melting point: 161°-162° C. The infrared absorption spectrum of this product was identical with that of the compound obtained in Example 34.

후처리

  1. temperaturethe mixture was refluxed for one hour
  2. customThe solvent was evaporated off
  3. additionthe addition of water
  4. extractionthe residue was extracted with ethyl acetate
  5. washThe ethyl acetate layer was washed with water
  6. dry with materialdried over Na2SO4
  7. customThe solvent was then evaporated off
  8. additionthe residue was treated with isopropyl ether

출처 및 근거

ORD 기록
ord-ce7514a5756e492dbd0762883753a63b
출처 데이터셋
uspto-grants-1979_04
특허 번호
US04150139

반응 노트

불러오는 중…