Hydroxylamine → HCID 23339651、化合物

HRID 28185ノート

反応式

HRID 28185 の反応式
[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

参加物

6

反応物 4

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

生成物 1

HCID 23339651HCID 23339651、化合物収率 62%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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 3N 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).

後処理

  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 3N HCl
  5. filtrationfiltered off
  6. washwashed with water
  7. customCRL 40,518 is obtained by recrystallisation from ethanol

出典と根拠

ORDレコード
ord-28ca8c3cfe154c77a663076b3c7e3729
出典データセット
uspto-grants-1980_09
特許番号
US04225617

反応ノート

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