2-Anisidine hydrochloride → 3-(2-Methoxyphenylaminomethylene)tetrahydropyran-2-one

HRID 729081ノート

反応式

HRID 729081 の反応式
[Na].O[CH:3]=[C:4]1[CH2:9][CH2:8][CH2:7][O:6][C:5]1=[O:10].Cl.[CH3:12][O:13][C:14]1[CH:20]=[CH:19][CH:18]=[CH:17][C:15]=1[NH2:16]>C(O)C>[CH3:12][O:13][C:14]1[CH:20]=[CH:19][CH:18]=[CH:17][C:15]=1[NH:16][CH:3]=[C:4]1[CH2:9][CH2:8][CH2:7][O:6][C:5]1=[O:10]

参加物

5

反応物 3

HCID 86382-Anisidine hydrochlorideHCID 5360545SodiumHCID 679061533-(Hydroxymethylene)-tetrahydropyran-2-one

生成物 1

HCID 542814473-(2-Methoxyphenylaminomethylene)tetrahydropyran-2-one収率 55%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

The sodium salt of 3-(hydroxymethylene)-tetrahydropyran-2-one (25 g, 0.17 mol) and 2-methoxyaniline hydrochloride (32 g, 0.2 mol) in ethanol (750 ml) were warmed to 70° C. with stirring for 2 hours, then filtered hot. After evaporation of the ethanol, the crude product was taken up in dichloromethane, washed with dilute hydrochloric acid, dried and evaporated. Trituration with ether gave 3-(2-methoxyphenylaminomethylene)tetrahydropyran-2-one (21.5 g, 55%) as a mixture of E and Z isomers, m.p. 85°-100°.

後処理

  1. filtrationfiltered hot
  2. customAfter evaporation of the ethanol
  3. washwashed with dilute hydrochloric acid
  4. customdried
  5. customevaporated

出典と根拠

ORDレコード
ord-36fdb4f109c94248b5012f9d2f4ca79c
出典データセット
uspto-grants-1991_09
特許番号
US05051508

反応ノート

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