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

HRID 26523노트

반응식

HRID 26523 반응식
CS([C:5]1[N:14]2[C:8]([CH2:9][C:10]3[CH:18]=[CH:17][CH:16]=[CH:15][C:11]=3[CH:12]=[CH:13]2)=[N:7][N:6]=1)(=O)=O.[CH3:19][O-:20].[Na+].CO>CO>[CH3:19][O:20][C:5]1[N:14]2[C:8]([CH2:9][C:10]3[CH:18]=[CH:17][CH:16]=[CH:15][C:11]=3[CH:12]=[CH:13]2)=[N:7][N:6]=1

참가 물질

4

반응물 2

HCID 213235253-methylsulfonyl-11H-s-triazolo[3,4-b][3]benzazapineHCID 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 0.522 g of 3-methylsulfonyl-11H-s-triazolo[3,4-b][3]benzazepine in 5 ml of methanol was added 3 ml of 2 N-sodium methoxide/methanol. The mixture was refluxed for 15 minutes and then the solvent was evaporated off. The residue was diluted with water and extracted with chloroform. The chloroform 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: 160°-161° C.

후처리

  1. temperatureThe mixture was refluxed for 15 minutes
  2. customthe solvent was evaporated off
  3. additionThe residue was diluted with water
  4. extractionextracted with chloroform
  5. washThe chloroform 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-a9d49ac76bfe42409466037a002bccaa
출처 데이터셋
uspto-grants-1979_04
특허 번호
US04150139

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