Hydroxylamine → HCID 23339651、化合物

HRID 1707026ノート

反応式

HRID 1707026 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 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)

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 3 N 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-cf5c231508404d56b0e853b92afab3c1
出典データセット
uspto-grants-1980_06
特許番号
US04209523

反応ノート

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