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Sodium Hydroxide → HCID 21101214, 화합물

HRID 1352851
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HRID 1352851 반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6](/[CH:9]=[CH:10]/[C:11](OCC)=[O:12])=[CH:5][C:4]=1[O:16][CH2:17][O:18][CH3:19].[OH-].[Na+]>C1(C)C=CC=CC=1.CCCCCC>[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6](/[CH:9]=[CH:10]/[CH2:11][OH:12])=[CH:5][C:4]=1[O:16][CH2:17][O:18][CH3:19]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 14798Sodium HydroxideHCID 89258928HCID 89258928, 화합물

생성물 1

HCID 21101214HCID 21101214, 화합물수율 95.7%

시약·촉매·용매 2

HCID 1140Toluene용매HCID 8058Hexane용매

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온도
-78 °C

실험 절차

A solution of the compound (4.54 g, 17.0 mmol) of Example 9-2 in toluene (60 ml) was stirred at −78° C., and thereto was dropped diisobutylalminumhydride (1.0M in hexane: 35.8 ml, 35.8 mmol). The mixture was stirred for 1.5 hours at −78° C., followed by addition of an aqueous 2N sodium hydroxide solution. The precipitate was filtered off and the filtrate was extracted with ethyl acetate. The organic layer was washed with water and an aqueous sodium chloride solution in the order, and dried over anhydrous magnesium sulfate. The solvent was removed under reduced pressure to give the subject compound (3.65 g, 95.7%).

후처리

  1. filtrationThe precipitate was filtered off
  2. extractionthe filtrate was extracted with ethyl acetate
  3. washThe organic layer was washed with water
  4. dry with materialan aqueous sodium chloride solution in the order, and dried over anhydrous magnesium sulfate
  5. customThe solvent was removed under reduced pressure

출처 및 근거

ORD 기록
ord-02cfd4d2298b4381a26ca2fb55c4e089
출처 데이터셋
uspto-grants-2007_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07220773B2

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