Acetic Acid → Gsk-269984B

HRID 2356614

반응식

HRID 2356614 반응식
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([O:18][CH2:19][C:20]2[CH:25]=[CH:24][C:23]([Cl:26])=[CH:22][C:21]=2[F:27])=[C:6]([CH2:8][C:9]2[N:14]=[C:13]([C:15]([O-:17])=[O:16])[CH:12]=[CH:11][CH:10]=2)[CH:7]=1.[Na+].O.C(O)(=O)C>C(OCC)(=O)C>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([O:18][CH2:19][C:20]2[CH:25]=[CH:24][C:23]([Cl:26])=[CH:22][C:21]=2[F:27])=[C:6]([CH2:8][C:9]2[N:14]=[C:13]([C:15]([OH:17])=[O:16])[CH:12]=[CH:11][CH:10]=2)[CH:7]=1

참가 물질

5

반응물 3

HCID 176Acetic AcidHCID 962WaterHCID 23696973Gsk-269984A

생성물 1

HCID 11495634Gsk-269984B

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

Sodium 6-[(5-chloro-2-{[(4-chloro-2-fluorophenyl)methyl]oxy}phenyl)methyl]-2-pyridinecarboxylate (3.0 g) was suspended in ethyl acetate (100 ml) and water (100 ml) with stirring. Acetic acid (1.0 ml) was added to give two clear phases which were separated. The ethyl acetate layer was dried over magnesium sulfate and concentrated to give an oil which crystallised after a few minutes. Toluene (100 ml) was added and the solution was re-evaporated to give a white solid. Left at 20 mBar for 5 hours at 45° C. 2.69 g.

후처리

  1. customto give two clear phases which
  2. customwere separated
  3. dry with materialThe ethyl acetate layer was dried over magnesium sulfate
  4. concentrationconcentrated
  5. customto give an oil which
  6. customcrystallised after a few minutes
  7. additionToluene (100 ml) was added
  8. customthe solution was re-evaporated
  9. customto give a white solid

출처 및 근거

ORD 기록
ord-2ab341abf424456fa9e9a31cb968789a
출처 데이터셋
uspto-grants-2010_07
특허 번호
US07759369B2

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