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Acetic Anhydride → 2-Acetoxymethyl-3-methyl-4-(2,2,2-trifluoroethoxy)pyridine

HRID 1444738
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HRID 1444738 반응식
[CH3:1][C:2]1[C:7]([CH3:8])=[C:6]([O:9][CH2:10][C:11]([F:14])([F:13])[F:12])[CH:5]=[CH:4][N+:3]=1[O-].[CH3:16][C:17]([O:19]C(C)=O)=[O:18]>C(Cl)Cl.CN(C)C1C=CN=CC=1>[C:17]([O:19][CH2:1][C:2]1[C:7]([CH3:8])=[C:6]([O:9][CH2:10][C:11]([F:14])([F:13])[F:12])[CH:5]=[CH:4][N:3]=1)(=[O:18])[CH3:16]
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참가 물질

5

반응물 2

HCID 7918Acetic AnhydrideHCID 111720662,3-Dimethyl-4-(2,2,2-trifluoroethoxy)pyridine 1-oxide

생성물 1

HCID 231348662-Acetoxymethyl-3-methyl-4-(2,2,2-trifluoroethoxy)pyridine수율 94%

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 6344Dichloromethane용매

반응 조건

온도
92.5 °C

실험 절차

40 ml of 2,3-dimethyl-4-(2,2,2-trifluoroethoxy)pyridine N-oxide (0.078 mole) in methylene chloride were dropwise added to a solution of 28.7 ml acetanhydride and 0.182 g 4-dimethylaminopyridine, then methylene chloride was distilled off and the residue was heated to a temperature of from 90 to 95° C. for 4-5 hours. At the end of the reaction, 3.6 ml of water were added and acetic acid was removed by vacuum distillation to obtain an oil product. The yield was 94-96%, determined by HPLC.

후처리

  1. distillationmethylene chloride was distilled off
  2. customAt the end of the reaction, 3.6 ml of water
  3. additionwere added
  4. customacetic acid was removed by vacuum distillation
  5. customto obtain an oil product

출처 및 근거

ORD 기록
ord-fce8178bd3c44bf89d8d4fe55baef065
출처 데이터셋
uspto-grants-2010_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07662968B2

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