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

HRID 26523ノート

反応式

HRID 26523 の反応式
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

参加物

4

反応物 2

HCID 213235253-methylsulfonyl-11H-s-triazolo[3,4-b][3]benzazapineHCID 23694274Sodium methanolate methanol

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-a9d49ac76bfe42409466037a002bccaa
出典データセット
uspto-grants-1979_04
特許番号
US04150139

反応ノート

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