Methyl iodide → 3-methylthio-11H-s-triazolo[3,4-b][3]benzazepine

HRID 26508

반응식

HRID 26508 반응식
[N:1]1[NH:2][C:3](=[S:15])[N:4]2[CH:10]=[CH:9][C:8]3[CH:11]=[CH:12][CH:13]=[CH:14][C:7]=3[CH2:6][C:5]=12.[CH3:16][O-].[Na+].CO.CI>CO>[CH3:16][S:15][C:3]1[N:4]2[C:5]([CH2:6][C:7]3[CH:14]=[CH:13][CH:12]=[CH:11][C:8]=3[CH:9]=[CH:10]2)=[N:1][N:2]=1

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 130724232,11-dihydro-3H-s-triazolo[3,4-b][3]benzazepine-3-thioneHCID 23694274Sodium methanolate methanol

생성물 1

HCID 213234063-methylthio-11H-s-triazolo[3,4-b][3]benzazepine

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To 3 ml of methanol was added 0.215 g of 2,11-dihydro-3H-s-triazolo[3,4-b][3]benzazepine-3-thione and, under stirring, 0.6 ml of 2N-sodium methoxide/methanol was added. Then, 0.07 ml of methyl iodide was added dropwise. After 20 minutes, the reaction mixture 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 ether. In this manner, 3-methylthio-11H-s-triazolo[3,4-b][3]benzazepine were obtained as crystals. Recrystallization from methanol yielded colorless needles melting at 168°-169° C. This was identical with the products obtained in Examples 1 and 2.

후처리

  1. extractionthe reaction mixture was extracted with ethyl acetate
  2. washThe ethyl acetate layer was washed with water
  3. dry with materialdried over Na2SO4
  4. customThe solvent was then evaporated off
  5. additionthe residue was treated with ether

출처 및 근거

ORD 기록
ord-bab0281336fd44af883de71d8461ae1f
출처 데이터셋
uspto-grants-1979_04
특허 번호
US04150139

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