Hydrochloric Acid → HCID 67926517, 화합물

HRID 981257노트

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HRID 981257 반응식
[C:1]([C:4]1[CH:44]=[CH:43][C:7]([O:8][CH2:9][CH2:10][CH2:11][S:12][C:13]2[CH:18]=[CH:17][C:16]([CH:19]([S:27][C:28]3[CH:33]=[CH:32][C:31]([C:34](=[O:42])[CH:35]([CH3:41])[CH2:36][C:37]([O:39]C)=[O:38])=[CH:30][CH:29]=3)[CH:20]([CH3:26])[CH2:21][C:22]([O:24]C)=[O:23])=[CH:15][CH:14]=2)=[C:6]([CH2:45][CH2:46][CH3:47])[C:5]=1[OH:48])(=[O:3])[CH3:2].CO.[OH-].[Na+].Cl>C1COCC1.O>[OH2:3].[C:1]([C:4]1[CH:44]=[CH:43][C:7]([O:8][CH2:9][CH2:10][CH2:11][S:12][C:13]2[CH:18]=[CH:17][C:16]([CH:19]([S:27][C:28]3[CH:29]=[CH:30][C:31]([C:34](=[O:42])[CH:35]([CH3:41])[CH2:36][C:37]([OH:39])=[O:38])=[CH:32][CH:33]=3)[CH:20]([CH3:26])[CH2:21][C:22]([OH:24])=[O:23])=[CH:15][CH:14]=2)=[C:6]([CH2:45][CH2:46][CH3:47])[C:5]=1[OH:48])(=[O:3])[CH3:2]

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 887MethanolHCID 14798Sodium HydroxideHCID 20071763HCID 20071763, 화합물

생성물 1

HCID 67926517HCID 67926517, 화합물수율 79%

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of ester from Step A of this Example (760 mg) in THF (15 ml) and MeOH (1 ml) was added 2N NaOH (2.4 ml) and stirred overnight at room temperature. The reaction mixture was diluted with H2O (50 ml) and acidified with 2N HCl and extracted with CH2Cl2 (2×50 ml). The combined organic layers were washed with brine, dried over Na2SO4 and purified on a column of flash silica gel 230-400 mesh using toluene-dioxane-acetic acid (10:2:0.1) as eluant to give the title compound as a foam (580 mg, 79%).

후처리

  1. extractionextracted with CH2Cl2 (2×50 ml)
  2. washThe combined organic layers were washed with brine
  3. dry with materialdried over Na2SO4
  4. custompurified on a column of flash silica gel 230-400 mesh

출처 및 근거

ORD 기록
ord-3e4ff46650eb4d4c93f9ead754d97bb9
출처 데이터셋
uspto-grants-1991_02
특허 번호
US04990526

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