3-Amino-4-hydroxybenzoic acid → 2-(4-Carbomethoxyphenyl)-5-carboxybenzoxazole

HRID 2419531

반응식

HRID 2419531 반응식
[CH3:1][O:2][C:3](=[O:14])[C:4]1[CH:9]=[CH:8][C:7]([C:10](Cl)(Cl)Cl)=[CH:6][CH:5]=1.[NH2:15][C:16]1[CH:17]=[C:18]([CH:22]=[CH:23][C:24]=1[OH:25])[C:19]([OH:21])=[O:20]>>[C:3]([C:4]1[CH:9]=[CH:8][C:7]([C:10]2[O:25][C:24]3[CH:23]=[CH:22][C:18]([C:19]([OH:21])=[O:20])=[CH:17][C:16]=3[N:15]=2)=[CH:6][CH:5]=1)([O:2][CH3:1])=[O:14]

참가 물질

3

반응물 2

HCID 650833-Amino-4-hydroxybenzoic acidHCID 84661Methyl 4-(trichloromethyl)benzoate

생성물 1

HCID 203138222-(4-Carbomethoxyphenyl)-5-carboxybenzoxazole

반응 조건

온도
200 °C

실험 절차

In the apparatus described in Example 1, 12.7 g of 4-trichloromethylbenzoic acid methyl ester (0.05 mol) and 7.5 g of 3-amino-4-hydroxybenzoic acid (0.05 mol) were mixed and heated for 6 hours at 200° C. The reaction product after grinding in a mortar was extracted twice with 100 ml of CHCl3 and then, after drying, twice with 100 ml of water. 9.2 g of raw product remained, melting at 275° to 284° C (62% of the theory). After two recrystallizations with dimethyl formamide plus active charcoal and dimethylsulfoxide, the melting point was 291° to 293° C.

후처리

  1. additionwere mixed
  2. customThe reaction product after grinding in a mortar
  3. extractionwas extracted twice with 100 ml of CHCl3
  4. dry with materialafter drying, twice with 100 ml of water
  5. customAfter two recrystallizations with dimethyl formamide plus active charcoal and dimethylsulfoxide

출처 및 근거

ORD 기록
ord-bf3bc6f118534e35b09056df7eca003b
출처 데이터셋
uspto-grants-1978_08
특허 번호
US04107169

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