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

HRID 729081노트

반응식

HRID 729081 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 542814473-(2-Methoxyphenylaminomethylene)tetrahydropyran-2-one수율 55%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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°.

후처리

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

출처 및 근거

ORD 기록
ord-36fdb4f109c94248b5012f9d2f4ca79c
출처 데이터셋
uspto-grants-1991_09
특허 번호
US05051508

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