Acetic Anhydride → N-[2-morpholin-4-yl-5-(trifluoromethyl)phenyl]acetamide

HRID 262011

반응식

HRID 262011 반응식
[NH2:1][C:2]1[CH:7]=[C:6]([C:8]([F:11])([F:10])[F:9])[CH:5]=[CH:4][C:3]=1[N:12]1[CH2:17][CH2:16][O:15][CH2:14][CH2:13]1.[C:18](OC(=O)C)(=[O:20])[CH3:19]>C(COC)OC>[C:18]([NH:1][C:2]1[CH:7]=[C:6]([C:8]([F:9])([F:10])[F:11])[CH:5]=[CH:4][C:3]=1[N:12]1[CH2:13][CH2:14][O:15][CH2:16][CH2:17]1)(=[O:20])[CH3:19]

참가 물질

4

반응물 2

HCID 7918Acetic AnhydrideHCID 136624N-(2-Amino-4-(trifluoromethyl)phenyl)morpholine

생성물 1

HCID 891590N-[2-morpholin-4-yl-5-(trifluoromethyl)phenyl]acetamide수율 96%

시약·촉매·용매 1

HCID 80711,2-Dimethoxyethane용매

실험 절차

A mixture of 40 g. (16 mmoles) of 4-(2-amino-4-trifluoromethylphenyl)morpholine and 2.2 g. (22 mmoles) of acetic anhydride in 40 ml. of dry dimethoxyethane was heated at 70° C. for 10 hours. The reaction mixture was cooled to room temperature and then the solvent removed by evaporation under reduced pressure. The residue was dissolved in 100 ml. of methylene chloride and the solution washed with 5% sodium bicarbonate solution. After drying over anhydrous sodium sulfate, the solution was filtered and evaporated under reduced pressure. The residue was dissolved in n-hexane from which it crystallized to give 4.4 g. (96%) of the desired product melting at 85° C.

후처리

  1. additionA mixture of 40 g
  2. customthe solvent removed by evaporation under reduced pressure
  3. dissolutionThe residue was dissolved in 100 ml
  4. washof methylene chloride and the solution washed with 5% sodium bicarbonate solution
  5. dry with materialAfter drying over anhydrous sodium sulfate
  6. filtrationthe solution was filtered
  7. customevaporated under reduced pressure
  8. dissolutionThe residue was dissolved in n-hexane from which it
  9. customcrystallized
  10. customto give 4.4 g

출처 및 근거

ORD 기록
ord-ce8cc36323974fc4a0b387a8ecfe63ce
출처 데이터셋
uspto-grants-1979_05
특허 번호
US04153443

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