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Hydrochloric Acid → 1-Cyano-2-hydroxy-1-(4-trifluoromethylphenyl)aminothiocarbonylpropene

HRID 1416540
ノート
印刷プレビュー

反応式

HRID 1416540 の反応式
[CH3:1][C:2]1[O:6][N:5]=[CH:4][C:3]=1[C:7]([NH:9][C:10]1[CH:15]=[CH:14][C:13]([C:16]([F:19])([F:18])[F:17])=[CH:12][CH:11]=1)=[S:8].N12CCCN=C1CCCCC2.Cl>C(O)C>[C:4]([C:3]([C:7]([NH:9][C:10]1[CH:15]=[CH:14][C:13]([C:16]([F:17])([F:18])[F:19])=[CH:12][CH:11]=1)=[S:8])=[C:2]([OH:6])[CH3:1])#[N:5]
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 3

HCID 313Hydrochloric AcidHCID 811841,8-Diazabicyclo(5.4.0)undec-7-eneHCID 158588075-Methyl-4-(4-trifluoromethylphenyl)aminothiocarbonylisoxazole

生成物 1

HCID 1363959891-Cyano-2-hydroxy-1-(4-trifluoromethylphenyl)aminothiocarbonylpropene収率 71.4%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of 7.0 grams of 5-methyl-4-(4-trifluoromethylphenyl)aminothiocarbonylisoxazole and 5 ml of 1,8-diazabicyclo[5.4.0]undec-7-ene in 50 ml of ethanol was heated at 80° C. for 8 hours. The reaction mixture was cooled to room temperature and acidified with 6N hydrochloric acid solution until pH 2. The mixture was then cooled in an ice-water bath for 30 minutes and the solid was filtered, washed with a chilled solution of ethanol and water (2:1) and dried by suction to provide 5.0 grams of 1-cyano-2-hydroxy-1-(4-trifluoromethylphenyl) aminothiocarbonylpropene.

後処理

  1. temperatureThe mixture was then cooled in an ice-water bath for 30 minutes
  2. filtrationthe solid was filtered
  3. washwashed with a chilled solution of ethanol and water (2:1)
  4. customdried by suction

出典と根拠

ORDレコード
ord-d6df24e2b5f348ac8c62e3c89570833d
出典データセット
uspto-grants-1999_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05914343

反応ノート

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