Hydrochloric Acid → HCID 49806002, 화합물

HRID 1615060노트

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HRID 1615060 반응식
[CH:1]1([C:4]2[CH:48]=[CH:47][C:7]([CH2:8][O:9][C:10]3[CH:15]=[CH:14][C:13]([CH:16]4[CH2:19][N:18]([C:20]([C:22]5[CH:27]=[C:26]([CH2:28][O:29][CH2:30][C:31]6([CH2:43][OH:44])[CH2:36][O:35]C(C7C=CC=CC=7)[O:33][CH2:32]6)[CH:25]=[CH:24][N:23]=5)=[O:21])[CH2:17]4)=[CH:12][C:11]=3[O:45][CH3:46])=[CH:6][CH:5]=2)[CH2:3][CH2:2]1.Cl.[OH-].[Na+].C([O-])(O)=O.[Na+]>O1CCCC1>[CH:1]1([C:4]2[CH:48]=[CH:47][C:7]([CH2:8][O:9][C:10]3[CH:15]=[CH:14][C:13]([CH:16]4[CH2:17][N:18]([C:20]([C:22]5[CH:27]=[C:26]([CH2:28][O:29][CH2:30][C:31]([CH2:32][OH:33])([CH2:36][OH:35])[CH2:43][OH:44])[CH:25]=[CH:24][N:23]=5)=[O:21])[CH2:19]4)=[CH:12][C:11]=3[O:45][CH3:46])=[CH:6][CH:5]=2)[CH2:2][CH2:3]1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 516892Sodium BicarbonateHCID 59634057HCID 59634057, 화합물2회

생성물 1

HCID 49806002HCID 49806002, 화합물수율 44%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of the crude {3-[4-(4-cyclopropylbenzyloxy)-3-methoxyphenyl]azetidin-1-yl}-[4-(5-hydroxymethyl-2-phenyl-[1,3]dioxan-5-ylmethoxymethyl)-pyridin-2-yl]-methanone prepared in (1) in THF (10 mL) was added 1 N hydrochloric acid (5.0 mL). The reaction mixture was stirred at RT for 24 hr. To the reaction mixture were added aqueous 1 N NaOH and saturated aqueous NaHCO3 and then the mixture was extracted with ethyl acetate. The organic layer was dried over MgSO4. The solvent was removed under reduced pressure. The residue was purified by silica gel chromatography (Developing solvent: chloroform/methanol=5/1) to give the title compound (0.33 g, 44%).

후처리

  1. extractionthe mixture was extracted with ethyl acetate
  2. dry with materialThe organic layer was dried over MgSO4
  3. customThe solvent was removed under reduced pressure
  4. customThe residue was purified by silica gel chromatography (Developing solvent: chloroform/methanol=5/1)

출처 및 근거

ORD 기록
ord-c5d4214a80404bf897b515c0be28a41c
출처 데이터셋
uspto-grants-2014_07
특허 번호
US08765739B2

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