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Hydroxylamine, O-(3-chloro-2-propenyl)-, hydrochloride → 2-[1-(3-Chloroallyloxyimino)propyl]-3-hydroxy-5-(3-crotonyl-2,4,6-trimethylphenyl)cyclohex-2-en-1-one

HRID 1906351
ノート
印刷プレビュー

反応式

HRID 1906351 の反応式
Cl.[Cl:2][CH:3]=[CH:4][CH2:5][O:6][NH2:7].C([O-])(=O)C.[Na+].[OH:13][C:14]1[CH2:19][CH:18]([C:20]2[C:25]([CH3:26])=[CH:24][C:23]([CH3:27])=[C:22]([C:28](=[O:32])/[CH:29]=[CH:30]/[CH3:31])[C:21]=2[CH3:33])[CH2:17][C:16](=[O:34])[C:15]=1[C:35](=O)[CH2:36][CH3:37]>C(O)C>[Cl:2][CH:3]=[CH:4][CH2:5][O:6][N:7]=[C:35]([C:15]1[C:14](=[O:13])[CH2:19][CH:18]([C:20]2[C:25]([CH3:26])=[CH:24][C:23]([CH3:27])=[C:22]([C:28](=[O:32])/[CH:29]=[CH:30]/[CH3:31])[C:21]=2[CH3:33])[CH2:17][C:16]=1[OH:34])[CH2:36][CH3:37]
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 158057Hydroxylamine, O-(3-chloro-2-propenyl)-, hydrochlorideHCID 517045Sodium AcetateHCID 178450140HCID 178450140、化合物

生成物 1

HCID 1363321822-[1-(3-Chloroallyloxyimino)propyl]-3-hydroxy-5-(3-crotonyl-2,4,6-trimethylphenyl)cyclohex-2-en-1-one収率 85%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

3-Chloroallyloxyamine hydrochloride (0.3 g) and then anhydrous sodium acetate (0.2 g) were added to a solution of 3-hydroxy-5-(3-crotonyl-2,4,6-trimethylphenyl)-2-propionylcyclohex-2-en-1-one (0.7 g) in anhydrous ethanol (80 ml). The mixture was stirred briefly then allowed to stand at room temperature for 16 hours. The ethanol was removed by evaporation under reduced pressure using a rotary evaporator. The residue was treated with chloroform and the organic phase was washed twice with water (50 ml). The chloroform layer was dried over magnesium sulphate and the solvent was removed by evaporation under reduced pressure to give the product 2-[1-(3-chloroallyloxyimino)propyl]-3-hydroxy-5-(3-crotonyl-2,4,6-trimethylphenyl)cyclohex-2-en-1-one (0.7 g, 85%) as a colourless oil. Proton magnetic spectrum (CDCl3 ; δ in ppm); 1.19 (3H, t); 1.92 (3H, d, J=7 Hz); 2.09 (3H, s); 2.19 (3H, s); 2.39 (3H, s); 2.2-4.0 (7H, m); 4.4-4.8 (2H, m); 5.86.7 (4H, m); 6.86 (1H, s); 15.2 (1 H, bs).

後処理

  1. customThe ethanol was removed by evaporation under reduced pressure
  2. customa rotary evaporator
  3. additionThe residue was treated with chloroform
  4. washthe organic phase was washed twice with water (50 ml)
  5. dry with materialThe chloroform layer was dried over magnesium sulphate
  6. customthe solvent was removed by evaporation under reduced pressure

出典と根拠

ORDレコード
ord-4d235abf22ff4279bf3c3715ecec8224
出典データセット
uspto-grants-1987_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04652303

反応ノート

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