Sodium Hydroxide → HCID 15230237, 화합물

HRID 234713

반응식

HRID 234713 반응식
C[O:2][C:3](=[O:33])[CH2:4][O:5][C:6]1[CH:15]=[CH:14][CH:13]=[C:12]2[C:7]=1[CH2:8][CH2:9][CH2:10][CH:11]2[C:16]([N:18]([CH2:26][C:27]1[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=1)[CH2:19][C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1)=[O:17].[OH-].[Na+]>C(COC)OC.CO>[CH2:26]([N:18]([CH2:19][C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1)[C:16]([CH:11]1[C:12]2[C:7](=[C:6]([O:5][CH2:4][C:3]([OH:33])=[O:2])[CH:15]=[CH:14][CH:13]=2)[CH2:8][CH2:9][CH2:10]1)=[O:17])[C:27]1[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=1

참가 물질

5

반응물 2

HCID 14798Sodium HydroxideHCID 15230236Methyl(1-dibenzylaminocarbonyl-1,2,3,4-tetrahydronaphthalen-5-yl)oxyacetate

생성물 1

HCID 15230237HCID 15230237, 화합물수율 86.6%

시약·촉매·용매 2

HCID 887Methanol용매HCID 80711,2-Dimethoxyethane용매

실험 절차

To a solution of the compound prepared in example 1 (204 mg) in dimethoxyethane (3 ml) and methanol (2 ml) was added 1N aqueous solution of sodium hydroxide. After stirred for 2 h, the mixture was quenched by addition of 1N hydrochloric acid. The mixture was extracted with ethyl acetate. The extract was washed with water and a saturated aqueous solution of sodium chloride, dried over anhydrous magnesium salfate, and evaporated. The residue was purified by silica gel column chromatography (ethyl acetate:hexane=1:4→ethyl acetate) to give the title compound (171 mg) having the following physical data.

후처리

  1. customthe mixture was quenched by addition of 1N hydrochloric acid
  2. extractionThe mixture was extracted with ethyl acetate
  3. washThe extract was washed with water
  4. dry with materiala saturated aqueous solution of sodium chloride, dried over anhydrous magnesium salfate
  5. customevaporated
  6. customThe residue was purified by silica gel column chromatography (ethyl acetate:hexane=1:4→ethyl acetate)

출처 및 근거

ORD 기록
ord-3a0c3e53415645eba0254c2e93098166
출처 데이터셋
uspto-grants-1997_01
특허 번호
US05596009

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