Hydrochloric Acid → Methyl 4-(2-oxopropyl)benzoate

HRID 580628

反応式

HRID 580628 の反応式
S(S([O-])(=O)=O)([O-])(=O)=[O:2].[Na+].[Na+].[C:11]([C:15]1[CH:20]=[CH:19][C:18]([CH2:21][C:22](=NO)[CH3:23])=[CH:17][CH:16]=1)([O:13][CH3:14])=[O:12].Cl>O.CO>[C:11]([C:15]1[CH:20]=[CH:19][C:18]([CH2:21][C:22](=[O:2])[CH3:23])=[CH:17][CH:16]=1)([O:13][CH3:14])=[O:12]

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 146045Sodium dithionateHCID 867397271-(4-Carbomethoxyphenyl)propan-2-one oxime

生成物 1

HCID 11137970Methyl 4-(2-oxopropyl)benzoate

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

Sodium metabisulphate (131 g) in water (300 ml) was added to 1-(4-carbomethoxyphenyl)propan-2-one oxime (37.5 g) in methanol (200 ml) and the mixture refluxed for 6 hours. The reaction mixture was cooled, concentrated hydrochloric acid (100 ml) added, the mixture extracted with chloroform and the combined chloroform extracts washed with water followed by sodium bicarbonate solution. The chloroform layer was dried (MgSO4) and evaporated to give the title compound as an oil (bp 126°-129°/0.7 mm) which crystallised on standing, (mp 40°-47°). τ (CDCl3) 7.88 (3H, s), 6.28 (2H, s), 6.14 (3H, s), 2.77 (2H, d, J=8 Hz), 2,04 (2H, d, J=8 Hz).

後処理

  1. temperaturethe mixture refluxed for 6 hours
  2. temperatureThe reaction mixture was cooled
  3. extractionthe mixture extracted with chloroform
  4. washthe combined chloroform extracts washed with water
  5. dry with materialThe chloroform layer was dried (MgSO4)
  6. customevaporated

出典と根拠

ORDレコード
ord-ace6e6a004ae49a58fec74cbc5e3bcce
出典データセット
uspto-grants-1988_06
特許番号
US04753962

関連ノート

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