Ethanol → 3-(4-Chlorophenyl)-2,1-benzisoxazole-7-acetic acid

HRID 1199021노트

반응식

HRID 1199021 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[O:9][N:10]=[C:11]3[C:16]([CH2:17][C:18]#N)=[CH:15][CH:14]=[CH:13][C:12]=23)=[CH:4][CH:3]=1.[OH-:20].[Na+].C(O)C.[OH2:25]>>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[O:9][N:10]=[C:11]3[C:16]([CH2:17][C:18]([OH:25])=[O:20])=[CH:15][CH:14]=[CH:13][C:12]=23)=[CH:4][CH:3]=1

참가 물질

5

반응물 4

HCID 702EthanolHCID 962WaterHCID 14798Sodium HydroxideHCID 156347583-(4-Chlorophenyl)-2,1-benzisoxazole-7-acetonitrile

생성물 1

HCID 156347603-(4-Chlorophenyl)-2,1-benzisoxazole-7-acetic acid수율 38%

실험 절차

A mixture of 3.9 g (0.015 mole) of 3-(4-chlorophenyl)-2,1-benzisoxazol-7-acetonitrile, 10 ml of 20% sodium hydroxide and 75 ml of 95% ethanol was heated at reflux under a nitrogen atmosphere for 17 hr. The mixture was poured into 600 ml of water and filtered. The filtrate was treated with charcoal and filtered through Celite. The filtrate was adjusted to pH 7 with concentrated hydrochloric acid and the mixture filtered. The filtrate was made acidic with concentrated hydrochloric acid and a solid precipitated. The solid was collected by filtration and recrystallized from 2-propanol to yield 1.6 g (38%) of pale-yellow needles, m.p. 200°-202° C. with decomposition.

후처리

  1. temperaturewas heated
  2. temperatureat reflux under a nitrogen atmosphere for 17 hr
  3. filtrationfiltered
  4. additionThe filtrate was treated with charcoal
  5. filtrationfiltered through Celite
  6. filtrationthe mixture filtered
  7. customa solid precipitated
  8. filtrationThe solid was collected by filtration
  9. customrecrystallized from 2-propanol

출처 및 근거

ORD 기록
ord-dee418807be844e18e44f3c1e906ceba
출처 데이터셋
uspto-grants-1990_02
특허 번호
US04898874

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