HCID 12213679, 화합물 → HCID 178482493, 화합물

HRID 2165737노트

반응식

HRID 2165737 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

HCID 178482493HCID 178482493, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-c2a05258086f44e29a52a9932875e788
출처 데이터셋
uspto-grants-1990_07
특허 번호
US04940790

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