Water → HCID 15359283, 화합물

HRID 1925521노트

반응식

HRID 1925521 반응식
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH:7]12[CH2:16][CH:11]3[CH2:12][CH:13]([CH2:15][CH:9]([CH2:10]3)[CH:8]1[CH2:17][C:18](OC)=[O:19])[CH2:14]2.O.[OH-].[Na+]>O1CCCC1>[CH:7]12[CH2:16][CH:11]3[CH2:12][CH:13]([CH2:15][CH:9]([CH2:10]3)[CH:8]1[CH2:17][CH2:18][OH:19])[CH2:14]2

참가 물질

6

반응물 4

HCID 962Water2회HCID 14798Sodium HydroxideHCID 21226445Aluminium lithium hydrideHCID 54117306Methyl 2-adamantylacetate

생성물 1

HCID 15359283HCID 15359283, 화합물수율 90%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

To a solution of lithium aluminium hydride (1.58 g, 41.63 mmol) in anhydrous tetrahydrofuran was slowly added a solution of Intermediate 72 (6.2 g, 29.76 mmol) in tetrahydrofuran (55 mL). The reaction mixture was stirred at room temperature overnight. Then water (12 mL), sodium hydroxide 4N (12 mL) and finally water again (36 mL) were added into the solution at 0° C. The mixture was stirred for some minutes and the resulting salts were filtered through a pad of Celite® washing with ethyl acetate (100 mL). The crude was treated with water and methylen chloride and the solvent of the organic layer was removed under reduced pressure to give the title compound as an oil (4.83 g, 90%), which was used in the next step without further purification.

후처리

  1. stirringThe mixture was stirred for some minutes
  2. filtrationthe resulting salts were filtered through a pad of Celite®
  3. washwashing with ethyl acetate (100 mL)
  4. additionThe crude was treated with water and methylen chloride
  5. customthe solvent of the organic layer was removed under reduced pressure

출처 및 근거

ORD 기록
ord-f6ef2fa6d30e4b5592c314d2f8cb18a7
출처 데이터셋
uspto-grants-2012_05
특허 번호
US08178679B2

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