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

HRID 2419531

反応式

HRID 2419531 の反応式
[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]

参加物

3

反応物 2

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

生成物 1

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

反応条件

温度
200 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-bf3bc6f118534e35b09056df7eca003b
出典データセット
uspto-grants-1978_08
特許番号
US04107169

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