3,6-Dimethyl-4-[(4-nitrophenyl)oxy]-1,2-benzisoxazole → {4-[(3,6-Dimethyl-1,2-benzisoxazol-4-yl)oxy]phenyl}amine

HRID 527521노트

반응식

HRID 527521 반응식
[CH3:1][C:2]1[C:6]2[C:7]([O:12][C:13]3[CH:18]=[CH:17][C:16]([N+:19]([O-])=O)=[CH:15][CH:14]=3)=[CH:8][C:9]([CH3:11])=[CH:10][C:5]=2[O:4][N:3]=1.O.O.[Sn](Cl)(Cl)(Cl)Cl>C(O)C>[CH3:1][C:2]1[C:6]2[C:7]([O:12][C:13]3[CH:18]=[CH:17][C:16]([NH2:19])=[CH:15][CH:14]=3)=[CH:8][C:9]([CH3:11])=[CH:10][C:5]=2[O:4][N:3]=1

참가 물질

4

반응물 2

HCID 679598393,6-Dimethyl-4-[(4-nitrophenyl)oxy]-1,2-benzisoxazole2회HCID 85782573Tin tetrachloride dihydrate

생성물 1

HCID 67960640{4-[(3,6-Dimethyl-1,2-benzisoxazol-4-yl)oxy]phenyl}amine수율 139.7%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

3,6-dimethyl-4-[(4-nitrophenyl)oxy]-1,2-benzisoxazole (Intermediate 20, 208 mg) was dissolved in ethanol (10.0 ml) and tin chloride dihydrate (991 mg, 4.39 mmol) was added. The reaction mixture was stirred and heated at reflux for 4 hours. After the removal of the volatiles, water was added and the reaction mixture was extracted two times with ethyl acetate. The collected organic were dried over sodium sulphate, filtered and evaporated to afford 260 mg of the title compound.

후처리

  1. temperatureheated
  2. temperatureat reflux for 4 hours
  3. customAfter the removal of the volatiles, water
  4. additionwas added
  5. extractionthe reaction mixture was extracted two times with ethyl acetate
  6. dry with materialThe collected organic were dried over sodium sulphate
  7. filtrationfiltered
  8. customevaporated

출처 및 근거

ORD 기록
ord-e39700682b174194a77c8d26339e2c7f
출처 데이터셋
uspto-grants-2016_05
특허 번호
US09346790B2

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