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

HRID 903635
ノート
印刷プレビュー

反応式

HRID 903635 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 312751,4-Dioxane溶媒

実験手順

900 mg of 9-cyano-2-methoxy-10,11-dihydro-11-oxo-dibenzo[b,f]thiepin was dissolved in the mixed solvent of 8 ml of ethanol and 8 ml of dioxane. To this was added 1.0 g 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 750 mg 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.

後処理

  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

出典と根拠

ORDレコード
ord-ddb4f147c9104fa180fc594dc7a296f9
出典データセット
uspto-grants-1980_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04228284

反応ノート

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