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

HRID 1112557

反応式

HRID 1112557 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 80711,2-Dimethoxyethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-e532cf478ac4487fbcef028a2aac72e7
出典データセット
uspto-grants-1978_10
特許番号
US04123251

関連ノート

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