Hydroxyamine hydrochloride → HCID 86736790、化合物

HRID 2052403ノート

反応式

HRID 2052403 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

HCID 86736790HCID 86736790、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-760bd40f43a84ba19089f0af03b233bf
出典データセット
uspto-grants-1980_01
特許番号
US04183951

反応ノート

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