Sodium borohydride → HCID 89852311, 화합물

HRID 627125노트

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HRID 627125 반응식
O.O.O.O.O.O.O.[Cl-].[Ce+3].[Cl-].[Cl-].[Si:12]([O:19][CH2:20][C@@H:21]1[C:26]([CH3:27])=[CH:25][C:24](=[O:28])[CH2:23][N:22]1[C:29]([O:31][C:32]([CH3:35])([CH3:34])[CH3:33])=[O:30])([C:15]([CH3:18])([CH3:17])[CH3:16])([CH3:14])[CH3:13].[BH4-].[Na+]>CO>[Si:12]([O:19][CH2:20][C@@H:21]1[C:26]([CH3:27])=[CH:25][C@H:24]([OH:28])[CH2:23][N:22]1[C:29]([O:31][C:32]([CH3:35])([CH3:34])[CH3:33])=[O:30])([C:15]([CH3:18])([CH3:16])[CH3:17])([CH3:14])[CH3:13]

참가 물질

5

반응물 3

HCID 4311764Sodium borohydrideHCID 21585214Cerium trichloride heptahydrateHCID 89852188(S)-tert-butyl 2-((tert-butyldimethylsilyloxy)methyl)-3-methyl-5-oxo-5,6-dihydropyridine-1 (2H)-carboxylate2회

생성물 1

HCID 89852311HCID 89852311, 화합물수율 90%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a stirred solution of cerium(III) chloride heptahydrate (6.36 g, 17.07 mmol) and (S)-tert-butyl 2-((tert-butyldimethylsilyloxy)methyl)-3-methyl-5-oxo-5,6-dihydropyridine-1(2H)-carboxylate (Intermediate 78, 6.07 g, 17.07 mmol) in MeOH (100 mL) at 0° C., sodium tetrahydroborate (0.646 g, 17.07 mmol) was added as a solid. The mixture was stirred at ambient temp for 1 h. The mixture was concentrated and diluted with NH4Cl(aq), H2O and extracted with ether. The ether layer was separated and washed with brine, dried over Na2SO4, filtered and concentrated to give the desired product (5.48 g, 90%) as a yellow oil.

후처리

  1. concentrationThe mixture was concentrated
  2. additiondiluted with NH4Cl(aq), H2O
  3. extractionextracted with ether
  4. customThe ether layer was separated
  5. washwashed with brine
  6. dry with materialdried over Na2SO4
  7. filtrationfiltered
  8. concentrationconcentrated

출처 및 근거

ORD 기록
ord-7e7b1b9bca3f4ad8b6d41aae16ec6d08
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09309245B2

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