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Hydroxyamine hydrochloride → alpha-(N-chloroacetyl-2-methyl-6-ethylphenylamino)acetaldehyde oxime

HRID 2286038
ノート
印刷プレビュー

反応式

HRID 2286038 の反応式
[Cl:1][CH2:2][C:3]([N:5]([C:9]1[C:14]([CH2:15][CH3:16])=[CH:13][CH:12]=[CH:11][C:10]=1[CH3:17])[CH2:6][CH:7]=O)=[O:4].Cl.[NH2:19][OH:20].C(=O)(O)[O-].[Na+]>C(O)C>[Cl:1][CH2:2][C:3]([N:5]([C:9]1[C:14]([CH2:15][CH3:16])=[CH:13][CH:12]=[CH:11][C:10]=1[CH3:17])[CH2:6][CH:7]=[N:19][OH:20])=[O:4]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 443297Hydroxyamine hydrochlorideHCID 516892Sodium BicarbonateHCID 20543832alpha-(N-chloroacetyl-2-methyl-6-ethylphenylamino)acetaldehyde

生成物 1

HCID 86736696alpha-(N-chloroacetyl-2-methyl-6-ethylphenylamino)acetaldehyde oxime収率 51.2%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of 5 g (0.2 mol) alpha-(N-chloroacetyl-2-methyl-6-ethylphenylamino)acetaldehyde, 3.3 g (0.04 mol) hydroxylamine hydrochloride and 3.4 g (0.04 mol) sodium bicarbonate in 50 ml ethanol was heated at 40° C. for 40 minutes. The reaction mixture was filtered, evaporated under reduced pressure, diluted with ethyl ether, filtered again and evaporated under reduced pressure to give 5.5 g of a yellow oil which crystallized to a solid on standing. The crude solid was recrystallized from ethyl ether/hexane to give 3.2 g of the product as a white solid, m.p. 113°-115° C. The product is tabulated in Table I as Compound No. 11.

後処理

  1. filtrationThe reaction mixture was filtered
  2. customevaporated under reduced pressure
  3. additiondiluted with ethyl ether
  4. filtrationfiltered again
  5. customevaporated under reduced pressure

出典と根拠

ORDレコード
ord-a35b33992f534fefa7bc58b4ea90a686
出典データセット
uspto-grants-1982_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04326077

反応ノート

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