Hydrochloric Acid → Methyl 4-(benzoxazol-2-yl)benzoate

HRID 2419530

反応式

HRID 2419530 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:21]=[CH:20][CH:19]=[CH:18][C:17]=1[OH:22].Cl>>[C:3]([C:4]1[CH:9]=[CH:8][C:7]([C:10]2[O:22][C:17]3[CH:18]=[CH:19][CH:20]=[CH:21][C:16]=3[N:15]=2)=[CH:6][CH:5]=1)([O:2][CH3:1])=[O:14]

参加物

4

反応物 3

HCID 313Hydrochloric AcidHCID 58012-AminophenolHCID 84661Methyl 4-(trichloromethyl)benzoate

生成物 1

HCID 650931Methyl 4-(benzoxazol-2-yl)benzoate

実験手順

In the apparatus described in Example 1, 25.4 g of 4-trichloromethylbenzoic acid methyl ester (0.1 mol) and 10.9 g of 2-aminophenol (0.1 mol) were mixed and slowly heated up to 200° C, so that the stream of HCl that commences at 130° C would not become too strong. The total reaction time was about 4 hours. The ground reaction product was washed thrice with 100 ml of hot benzene and the combined and concentrated benzene phases where chromatographed through an Al2O3 : 8.9 g of raw product XVI, melting point 190°-191° C (35% of the theory), becoming 193°-194° C after recrystallization from benzene.

後処理

  1. additionwere mixed
  2. customThe ground reaction product
  3. washwas washed thrice with 100 ml of hot benzene
  4. customthe combined and concentrated benzene phases where chromatographed through an Al2O3
  5. custombecoming 193°-194° C
  6. customafter recrystallization from benzene

出典と根拠

ORDレコード
ord-5bd137bfe13f40e9b8901c42f2d4f155
出典データセット
uspto-grants-1978_08
特許番号
US04107169

関連ノート

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