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

HRID 26496
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HRID 26496 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-b2a796f2b1ed403fa68ebf793d57b8b8
출처 데이터셋
uspto-grants-1979_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04150139

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