Hydrochloric Acid → 3-Chloro-5-hydroxy-1-iodo-2-[3-(5-trifluoromethylpyrid-2-yloxy)propyloxy]-benzene

HRID 497052노트

반응식

HRID 497052 반응식
C([O:9][C:10]1[CH:11]=[C:12]([Cl:32])[C:13]([O:17][CH2:18][CH2:19][CH2:20][O:21][C:22]2[CH:27]=[CH:26][C:25]([C:28]([F:31])([F:30])[F:29])=[CH:24][N:23]=2)=[C:14]([I:16])[CH:15]=1)(=O)C1C=CC=CC=1.[OH-].[Na+].Cl>O1CCCC1.CO>[Cl:32][C:12]1[C:13]([O:17][CH2:18][CH2:19][CH2:20][O:21][C:22]2[CH:27]=[CH:26][C:25]([C:28]([F:31])([F:29])[F:30])=[CH:24][N:23]=2)=[C:14]([I:16])[CH:15]=[C:10]([OH:9])[CH:11]=1

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 223186095-Benzoyloxy-3-chloro-1-iodo-2-[3-(5-trifluoromethylpyrid-2-yloxy)propyloxy]benzene

생성물 1

HCID 223186173-Chloro-5-hydroxy-1-iodo-2-[3-(5-trifluoromethylpyrid-2-yloxy)propyloxy]-benzene

시약·촉매·용매 2

HCID 887Methanol용매HCID 8028Tetrahydrofuran용매

실험 절차

3.12 g of 5-benzoyloxy-3-chloro-1-iodo-2-[3-(5-trifluoromethylpyrid-2-yloxy)propyloxy]benzene were dissolved in 16 ml of tetrahydrofuran and 7.8 ml of methanol, and 3.9 ml of 2N aqueous sodium hydroxide solution were added. After 30 minutes of stirring at room temperature. 3.9 ml of 2N hydrochloric acid were added, and the reaction mixture was concentrated under reduced pressure. Saturated sodium chloride solution and ethyl acetate were added to the residue, and the mixture was shaken. The ethyl acetate phase was isolated, dried and concentrated. The resulting crude product was purified chromatographically. Yield: 2.03 g (80%)

후처리

  1. concentrationthe reaction mixture was concentrated under reduced pressure
  2. additionSaturated sodium chloride solution and ethyl acetate were added to the residue
  3. stirringthe mixture was shaken
  4. customThe ethyl acetate phase was isolated
  5. customdried
  6. concentrationconcentrated
  7. customThe resulting crude product was purified chromatographically

출처 및 근거

ORD 기록
ord-0b1f00f0866c4f468d1216b30b5bd9f7
출처 데이터셋
uspto-grants-2005_09
특허 번호
US06949551B2

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