Water → HCID 59506829, 화합물

HRID 250692

반응식

HRID 250692 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][CH2:9][C:10]([F:13])([F:12])[F:11])=[C:4]([F:14])[CH:3]=1.C([Li])CCC.CN(C)[CH:22]=[O:23].O>C1COCC1.C(=O)=O.CC(C)=O>[Cl:1][C:2]1[C:3]([CH:22]=[O:23])=[C:4]([F:14])[C:5]([O:8][CH2:9][C:10]([F:12])([F:11])[F:13])=[CH:6][CH:7]=1

참가 물질

7

반응물 4

HCID 962WaterHCID 6228DimethylformamideHCID 595067484-Chloro-2-fluoro-1-(2,2,2-trifluoroethoxy)benzeneHCID 178418339Butyllithium

생성물 1

HCID 59506829HCID 59506829, 화합물

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매HCID 18522661Acetone cardice용매

실험 절차

To 4-Chloro-2-fluoro-1-(2,2,2-trifluoro-ethoxy)-benzene (522, 0.80 g, 3.5 mmol) in THF (20 mL), cooled in dry ice/acetone bath and under an atmosphere of nitrogen, was slowly added n-butyllithium (1.60 M in Hexane, 2.30 mL). After an hour, N,N-dimethylformamide (0.298 mL, 3.85 mmol) was added to the reaction. After 30 minutes, the reaction was allowed to reach room temperature and was stirred for 10 minutes. The reaction was poured into water and extracted with ethyl acetate. The organic layer was dried over anhydrous sodium sulfate and filtered. The filtrate was concentrated and purified by silica gel column chromatography eluting with 20% ethyl acetate in hexane to give the compound (523, 450 mg, 50%).

후처리

  1. waitAfter an hour
  2. customto reach room temperature
  3. extractionextracted with ethyl acetate
  4. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  5. filtrationfiltered
  6. concentrationThe filtrate was concentrated
  7. custompurified by silica gel column chromatography
  8. washeluting with 20% ethyl acetate in hexane
  9. customto give the compound (523, 450 mg, 50%)

출처 및 근거

ORD 기록
ord-22949da1191b41feaab46b63d8d4a5de
출처 데이터셋
uspto-grants-2011_01
특허 번호
US07863288B2

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