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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Hydroxyamine hydrochloride → Acetamide, 2-((3,4-dichlorophenyl)amino)-N-hydroxy-

HRID 28178
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HRID 28178 반응식
C[O-].[Na+].[Na].Cl.[NH2:6][OH:7].[Cl:8][C:9]1[CH:10]=[C:11]([CH:19]=[CH:20][C:21]=1[Cl:22])[NH:12][CH2:13][C:14](OCC)=[O:15]>CO>[Cl:8][C:9]1[CH:10]=[C:11]([CH:19]=[CH:20][C:21]=1[Cl:22])[NH:12][CH2:13][C:14]([NH:6][OH:7])=[O:15]
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참가 물질

6

반응물 4

HCID 443297Hydroxyamine hydrochlorideHCID 2727804Ethyl 2-(3,4-dichloroanilino)acetateHCID 5360545SodiumHCID 10942334Sodium Methoxide

생성물 1

HCID 203276Acetamide, 2-((3,4-dichlorophenyl)amino)-N-hydroxy-수율 36%

시약·촉매·용매 1

HCID 887Methanol
용매
2회

실험 절차

A solution of sodium methylate, that is to say 3.22 g (0.14 gram atom) of sodium in 75 ml of methanol is mixed in the cold with 4.9 g (0.07 mol) of hydroxylamine hydrochloride in solution in 100 ml of methanol, the sodium chloride is filtered off and 16.1 g (0.065 mol) of ethyl 3,4-dichloroanilinoacetate are added to the filtrate. The reactants are left in contact overnight, the mixture is evaporated to dryness in vacuo, the residue is taken up with water, the solution is filtered over charcoal and the product is precipitated with 3 N HCl and filtered off. Recrystallisation from ethyl acetate gives CRL 40,500. Melting point=138°-140° C. (with decomposition). Yield: 36%.

후처리

  1. filtrationthe sodium chloride is filtered off
  2. customthe mixture is evaporated to dryness in vacuo
  3. filtrationthe solution is filtered over charcoal
  4. customthe product is precipitated with 3 N HCl
  5. filtrationfiltered off
  6. customRecrystallisation from ethyl acetate
  7. customgives CRL 40,500

출처 및 근거

ORD 기록
ord-c49840422d1549da8c2c43a802169c23
출처 데이터셋
uspto-grants-1980_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04225617

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