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

HRID 2419530

반응식

HRID 2419530 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: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]

참가 물질

4

반응물 3

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

생성물 1

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

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-5bd137bfe13f40e9b8901c42f2d4f155
출처 데이터셋
uspto-grants-1978_08
특허 번호
US04107169

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