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

HRID 26508

反応式

HRID 26508 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-bab0281336fd44af883de71d8461ae1f
出典データセット
uspto-grants-1979_04
特許番号
US04150139

関連ノート

読み込み中…