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2,11-dihydro-3H-s-triazolo[3,4-b][3]benzazepin-3-one → 2,5,6,11-tetrahydro-3H-s-triazolo[3,4-b][3]benzazepin-3-one

HRID 1414724
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인쇄 미리보기

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HRID 1414724 반응식
[N:1]1[NH:2][C:3](=[O: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>[Pd].C(O)(=O)C>[N:1]1[NH:2][C:3](=[O:15])[N:4]2[CH2:10][CH2:9][C:8]3[CH:11]=[CH:12][CH:13]=[CH:14][C:7]=3[CH2:6][C:5]=12
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

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

생성물 1

HCID 214850482,5,6,11-tetrahydro-3H-s-triazolo[3,4-b][3]benzazepin-3-one

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 176Acetic Acid용매

실험 절차

A mixture of 20 parts of 2,11-dihydro-3H-s-triazolo[3,4-b][3]benzazepin-3-one, 400 volume parts of acetic acid and 15 parts of 5% palladium-on-carbon is hydrogenated at atmospheric pressure and temperature under stirring. After 2600 volume parts of hydrogen is absorbed, the catalyst is removed by filtration. The filtrate is concentrated under reduced pressure and the residue is treated with diethyl ether to give 2,5,6,11-tetrahydro-3H-s-triazolo[3,4-b][3]benzazepin-3-one as crystals. Recrystallization from ethanol gives colorless plates melting at 253° - 261° C.

후처리

  1. customAfter 2600 volume parts of hydrogen is absorbed
  2. customthe catalyst is removed by filtration
  3. concentrationThe filtrate is concentrated under reduced pressure
  4. additionthe residue is treated with diethyl ether

출처 및 근거

ORD 기록
ord-8a28d2ae969b4584b524966e12487cba
출처 데이터셋
uspto-grants-1977_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04002638

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