Methanol → methyl 6-chloro-3,4-dihydro-2-methyl-3-oxo-2H-1,4-benzoxazine-8-carboxylate

HRID 329711

반응식

HRID 329711 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([C:14]([OH:16])=[O:15])[C:5]2[O:10][CH:9]([CH3:11])[C:8](=[O:12])[NH:7][C:6]=2[CH:13]=1.S(=O)(=O)(O)O.[CH3:22]O>>[Cl:1][C:2]1[CH:3]=[C:4]([C:14]([O:16][CH3:22])=[O:15])[C:5]2[O:10][CH:9]([CH3:11])[C:8](=[O:12])[NH:7][C:6]=2[CH:13]=1

참가 물질

4

반응물 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 145172316-chloro-3,4-dihydro-2-methyl-3-oxo-2H-1,4-benzoxazine-8-carboxylic acid

생성물 1

HCID 14517232methyl 6-chloro-3,4-dihydro-2-methyl-3-oxo-2H-1,4-benzoxazine-8-carboxylate

실험 절차

A mixture of 10 g of 6-chloro-3,4-dihydro-2-methyl-3-oxo-2H-1,4-benzoxazine-8-carboxylic acid, 150 ml of methanol and 5 ml of concentrated sulfuric acid is refluxed under heating with stirring for 40 hours, and then cooled. The precipitated crystals are collected by filtration, washed with methanol and dried to give 9.5 g of methyl 6-chloro-3,4-dihydro-2-methyl-3-oxo-2H-1,4-benzoxazine-8-carboxylate, melting at 186°-189° C.

후처리

  1. temperatureis refluxed
  2. temperatureunder heating
  3. temperaturecooled
  4. filtrationThe precipitated crystals are collected by filtration
  5. washwashed with methanol
  6. customdried

출처 및 근거

ORD 기록
ord-8d512f9f3219429ea838104cdff9ba23
출처 데이터셋
uspto-grants-1990_01
특허 번호
US04892872

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