HCID 12213679、化合物 → HCID 178482493、化合物

HRID 2165737ノート

反応式

HRID 2165737 の反応式
[Cl:1][CH2:2][C:3]([C:5]1[CH:10]=[C:9]([C:11]([CH3:14])([CH3:13])[CH3:12])[C:8]([OH:15])=[C:7]([C:16]([CH3:19])([CH3:18])[CH3:17])[CH:6]=1)=O.Cl.[CH3:21][NH:22][C:23](=[S:26])[NH:24][NH2:25]>C(O)C>[ClH:1].[C:16]([C:7]1[CH:6]=[C:5]([C:3]2[CH2:2][S:26][C:23]([NH:22][CH3:21])=[N:24][N:25]=2)[CH:10]=[C:9]([C:11]([CH3:14])([CH3:13])[CH3:12])[C:8]=1[OH:15])([CH3:19])([CH3:18])[CH3:17]

参加物

4

反応物 2

HCID 12213679HCID 12213679、化合物HCID 142109772-Chloro-1-(3,5-di-tert-butyl-4-hydroxyphenyl)ethan-1-one

生成物 1

HCID 178482493HCID 178482493、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

10.7 g (0.038 mol) of 2-chloro-1-(3,5-di-tert.butyl-4-hydroxyphenyl)-ethanone from step (a) and 4.8 g (0.034 mol) of 4-methylthiosemicarbazide hydrochloride were dissolved in 120 ml of ethanol, and the mixture was heated to boiling for 30 minutes. After cooling, the solvent was removed by distillation under reduced pressure, and the resinous residue was dissolved in 60 ml of warm ethyl acetate. On standing, the product immediately precipitated in crystalline form, and was filtered off and recrystallized again from 150 ml of a mixture of ethyl acetate and methylene chloride (10 : 1).

後処理

  1. temperaturethe mixture was heated
  2. temperatureAfter cooling
  3. customthe solvent was removed by distillation under reduced pressure
  4. dissolutionthe resinous residue was dissolved in 60 ml of warm ethyl acetate
  5. customthe product immediately precipitated in crystalline form
  6. filtrationwas filtered off
  7. customrecrystallized again from 150 ml of a mixture of ethyl acetate and methylene chloride (10 : 1)

出典と根拠

ORDレコード
ord-c2a05258086f44e29a52a9932875e788
出典データセット
uspto-grants-1990_07
特許番号
US04940790

反応ノート

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