Water → Acetanilide, 3'-acetyl-2,2,2-trifluoro-

HRID 230706

반응식

HRID 230706 반응식
[NH2:1][C:2]1[CH:3]=[C:4]([C:8](=[O:10])[CH3:9])[CH:5]=[CH:6][CH:7]=1.[F:11][C:12]([F:18])([F:17])[C:13](OC)=[O:14].O>CO>[C:8]([C:4]1[CH:3]=[C:2]([NH:1][C:13](=[O:14])[C:12]([F:18])([F:17])[F:11])[CH:7]=[CH:6][CH:5]=1)(=[O:10])[CH3:9]

참가 물질

5

반응물 3

HCID 962WaterHCID 74173'-AminoacetophenoneHCID 9893Methyl trifluoroacetate

생성물 1

HCID 673706Acetanilide, 3'-acetyl-2,2,2-trifluoro-수율 85%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

10 mmol of 3′-aminoacetophenone as a starting material was dissolved in a methanol solvent in a 100 mL round-bottomed flask and 1.2 equivalents (eq) of methyl trifluoroacetate was added dropwise thereto over 30 minutes at room temperature, and subsequently the reaction mixture was stirred for 2 hours. After the completion of the reaction was confirmed by TLC, a small amount of water was added to terminate the reaction. Then, the solvent was removed under reduced pressure. The residue was dissolved in 50 mL of ethyl acetate and washed twice with 30 mL of water, dried over anhydrous sodium sulfate, and distilled under reduced pressure to obtain the desired 3-acetyl-trifluoroacetylaminobenzene (85%) as a brown oil.

후처리

  1. customto terminate
  2. customthe reaction
  3. customThen, the solvent was removed under reduced pressure
  4. dissolutionThe residue was dissolved in 50 mL of ethyl acetate
  5. washwashed twice with 30 mL of water
  6. dry with materialdried over anhydrous sodium sulfate
  7. distillationdistilled under reduced pressure

출처 및 근거

ORD 기록
ord-765ccfd9ba554e248b48d58848b357ce
출처 데이터셋
uspto-grants-2009_07
특허 번호
US07566773B2

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