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Ethylene Glycol → 2,11-dihydro-3H-s-triazolo[3,4-b][3]benzazepin-3-one

HRID 26496
ノート
印刷プレビュー

反応式

HRID 26496 の反応式
[CH2:1]([OH:4])CO.[OH-].[K+].CSC1[N:18]2[C:12]([CH2:13][C:14]3[CH:22]=[CH:21][CH:20]=[CH:19][C:15]=3[CH:16]=[CH:17]2)=[N:11][N:10]=1.Cl>O>[N:11]1[NH:10][C:1](=[O:4])[N:18]2[CH:17]=[CH:16][C:15]3[CH:19]=[CH:20][CH:21]=[CH:22][C:14]=3[CH2:13][C:12]=12
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 174Ethylene GlycolHCID 313Hydrochloric AcidHCID 14797Potassium HydroxideHCID 213234063-methylthio-11H-s-triazolo[3,4-b][3]benzazepine

生成物 1

HCID 130667602,11-dihydro-3H-s-triazolo[3,4-b][3]benzazepin-3-one

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To 2 ml of ethylene glycol was added 0.2 g of potassium hydroxide, followed by addition of 0.23 g of 3-methylthio-11H-s-triazolo[3,4-b][3]benzazepine. The mixture was stirred at 150°-160° C. for 2 hours, after which water was added. The mixture was made acidic with 4N-hydrochloric acid and extracted with chloroform. The chloroform layer was washed with water and dried over Na2SO4. The solvent was evaporated off and the residue was treated with ethyl acetate. By the above procedure was obtained 2,11-dihydro-3H-s-triazolo[3,4-b][3]benzazepin-3-one as crystals. Recrystallization from methanol yielded light-brown needles melting at 207°-208° C. The following compounds were produced by procedures similar to that of the above Reference Example.

後処理

  1. extractionextracted with chloroform
  2. washThe chloroform layer was washed with water
  3. dry with materialdried over Na2SO4
  4. customThe solvent was evaporated off
  5. additionthe residue was treated with ethyl acetate

出典と根拠

ORDレコード
ord-b2a796f2b1ed403fa68ebf793d57b8b8
出典データセット
uspto-grants-1979_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04150139

反応ノート

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