Ammonia → 6-chloro-3,4-dihydro-2-methyl-3-oxo-2H-1,4-benzoxazine-8-carboxylic acid

HRID 329710

반응식

HRID 329710 반응식
[C:1]([C:4]1[CH:15]=[C:14]([Cl:16])[CH:13]=[C:12]([N+:17]([O-])=O)[C:5]=1[O:6][CH:7]([CH3:11])[C:8](O)=[O:9])([OH:3])=[O:2].N>O>[Cl:16][C:14]1[CH:15]=[C:4]([C:1]([OH:3])=[O:2])[C:5]2[O:6][CH:7]([CH3:11])[C:8](=[O:9])[NH:17][C:12]=2[CH:13]=1

참가 물질

4

반응물 2

HCID 222Ammonia2회HCID 145172302-(2-Carboxy-4-chloro-6-nitrophenoxy)propionic acid

생성물 1

HCID 145172316-chloro-3,4-dihydro-2-methyl-3-oxo-2H-1,4-benzoxazine-8-carboxylic acid수율 92.2%

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

To a solution of 960 g of ferrous sulfate heptahydrate in 2 1 of hot water is added a solution of 130 g of 2-(2-carboxy-4-chloro-6-nitrophenoxy)propionic acid and 200 ml of aqueous concentrated ammonia solution in 480 ml of water under stirring. After stirring for 30 minutes, to the reaction mixture is twice added 480 ml of aqueous concentrated ammonia solution. While the reaction mixture becomes exothermic, stirring is continued for an hour. The resultant mixture is filtered through a celite layer under reduced pressure and washed with 2 1 of hot water twice. The filtrate is cooled and made acid with concentrated hydrochloric acid. The precipitated crystals are washed with water and dried to give 100 g of 6-chloro-3,4-dihydro-2 -methyl-3-oxo-2H-1,4-benzoxazine-8-carboxylic acid, melting at 319°-320° C. with decomposition.

후처리

  1. stirringAfter stirring for 30 minutes, to the reaction mixture
  2. stirringstirring
  3. waitis continued for an hour
  4. filtrationThe resultant mixture is filtered through a celite layer under reduced pressure
  5. washwashed with 2 1 of hot water twice
  6. temperatureThe filtrate is cooled
  7. washThe precipitated crystals are washed with water
  8. customdried

출처 및 근거

ORD 기록
ord-d0cff010fc964bb5993de023b74ae6f4
출처 데이터셋
uspto-grants-1990_01
특허 번호
US04892872

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