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Hydrazine hydrate (1:1) → 9-Cyano-2-methoxy-10,11-dihydro-11-oxo-dibenzo[b,f]thiepin hydrazone

HRID 866915
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HRID 866915 반응식
[C:1]([C:3]1[C:8]2[CH2:9][C:10](=O)[C:11]3[CH:17]=[C:16]([O:18][CH3:19])[CH:15]=[CH:14][C:12]=3[S:13][C:7]=2[CH:6]=[CH:5][CH:4]=1)#[N:2].O.[NH2:22][NH2:23]>C(O)C.O1CCOCC1>[C:1]([C:3]1[C:8]2[CH2:9][C:10](=[N:22][NH2:23])[C:11]3[CH:17]=[C:16]([O:18][CH3:19])[CH:15]=[CH:14][C:12]=3[S:13][C:7]=2[CH:6]=[CH:5][CH:4]=1)#[N:2]
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참가 물질

5

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 126871079-Cyano-2-methoxy-10,11-dihydro-11-oxo-dibenzo[b,f]thiepin

생성물 1

HCID 867358609-Cyano-2-methoxy-10,11-dihydro-11-oxo-dibenzo[b,f]thiepin hydrazone수율 79.4%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 312751,4-Dioxane용매

실험 절차

900mg of 9-cyano-2-methoxy-10,11-dihydro-11-oxo-dibenzo-[b,f]thiepin was dissolved in the mixed solvent of 8ml of ethanol and 8ml of dioxane. To this was added 1.0g of 100% hydrazine hydrate and the resulting mixture was refluxed with stirring for 7.5 hours. After the completion of reaction, the solvent was distilled off to obtain the residue, which was washed with a small amount of ethanol, and there was obtained 750mg of 9-cyano-2-methoxy-10,11-dihydro-11-oxo-dibenzo[b,f]thiepin hydrazone as colorless needles having a melting point of 186°-187° C.

후처리

  1. temperaturethe resulting mixture was refluxed
  2. customAfter the completion of reaction
  3. distillationthe solvent was distilled off
  4. customto obtain the residue, which
  5. washwas washed with a small amount of ethanol

출처 및 근거

ORD 기록
ord-3761bb5d5ac64d35a86bc4e7edf3dde1
출처 데이터셋
uspto-grants-1978_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04101667

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