Hydroxyamine hydrochloride → HCID 86736790, 화합물

HRID 2052403노트

반응식

HRID 2052403 반응식
[Na].Cl.[NH2:3][OH:4].[CH3:5][O:6][C:7]1[CH:8]=[C:9]([NH:17][C:18]([CH2:20][C:21](OCC)=[O:22])=[O:19])[CH:10]=[C:11]([O:15][CH3:16])[C:12]=1[O:13][CH3:14]>CO>[CH3:5][O:6][C:7]1[CH:8]=[C:9]([OH:4])[CH:10]=[C:11]([O:15][CH3:16])[C:12]=1[O:13][CH3:14].[C:18]([CH2:20][C:21]([NH:3][OH:4])=[O:22])(=[O:19])[NH2:17]

참가 물질

5

반응물 3

HCID 443297Hydroxyamine hydrochlorideHCID 5360545SodiumHCID 54077321Ethyl 3,4,5-trimethoxyphenylcarbamoylacetate

생성물 1

HCID 86736790HCID 86736790, 화합물

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

4.15 g (0.18 gram atom) of sodium are added in small pieces to 100 ml of anhydrous methanol and this cold solution is then poured into a solution of 7 g (0.1 mol) of hydroxylamine hydrochloride in 100 ml of methanol; the sodium chloride is filtered off and 23.8 g (0.08 mol) of ethyl 3,4,5-trimethoxyphenylcarbamoylacetate 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 in water, the solution is acidified with 3 N HCl and the product is filtered off and washed with cold water and with diisopropyl ether. recrystallisation from methanol gives CRL 40,509. Melting point=195°-196° C. (with decomposition).

후처리

  1. filtrationthe sodium chloride is filtered off
  2. customthe mixture is evaporated to dryness in vacuo
  3. filtrationthe product is filtered off
  4. washwashed with cold water and with diisopropyl ether
  5. customrecrystallisation from methanol
  6. customgives CRL 40,509

출처 및 근거

ORD 기록
ord-760bd40f43a84ba19089f0af03b233bf
출처 데이터셋
uspto-grants-1980_01
특허 번호
US04183951

반응 노트

불러오는 중…