Hydroxylamine → HCID 23339651, 화합물

HRID 26816노트

반응식

HRID 26816 반응식
[C:1]1([NH:11][C:12]([CH2:14][C:15]([O:17]CC)=O)=[O:13])[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][CH:2]=1.[NH2:20][OH:21].Cl.NO.[Na]>CO>[C:1]1([NH:11][C:12]([CH2:14][C:15]([NH:20][OH:21])=[O:17])=[O:13])[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][CH:2]=1

참가 물질

6

반응물 4

HCID 787HydroxylamineHCID 443297Hydroxyamine hydrochlorideHCID 5360545SodiumHCID 12547460Ethyl alpha-naphthylcarbamoylacetate

생성물 1

HCID 23339651HCID 23339651, 화합물수율 62%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

19.3 g (0.075 mol) of ethyl α-naphthylcarbamoylacetate are treated with a solution of hydroxylamine, prepared from 5.6 g (0.08 mol) of hydroxylamine hydrochloride and 3.68 g of sodium in 250 ml of methanol. After leaving the reactants in contact for 5 hours, the mixture is evaporated to dryness in vacuo, the residue is taken up in 400 ml of cold water, the solution is filtered over charcoal, and the product is precipitated cold with 3 N HCl, filtered off and washed with water. CRL 40,518 is obtained by recrystallisation from ethanol. Yield: 62%. Melting point: 184°-186° C. (with decomposition).

후처리

  1. customAfter leaving the reactants in contact for 5 hours
  2. customthe mixture is evaporated to dryness in vacuo
  3. filtrationthe solution is filtered over charcoal
  4. customthe product is precipitated cold with 3 N HCl
  5. filtrationfiltered off
  6. washwashed with water
  7. customCRL 40,518 is obtained by recrystallisation from ethanol

출처 및 근거

ORD 기록
ord-34e19f4dc75d49fc88b2096e844cd957
출처 데이터셋
uspto-grants-1979_04
특허 번호
US04151300

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