Water → HCID 70144159, 화합물

HRID 496071노트

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HRID 496071 반응식
[BH4-].[Li+].[C:3]([O:7][C:8]([N:10]([CH3:19])[C:11]1([CH2:14][C:15](OC)=[O:16])[CH2:13][CH2:12]1)=[O:9])([CH3:6])([CH3:5])[CH3:4].O.C(=O)([O-])[O-].[Na+].[Na+]>O1CCCC1>[OH:16][CH2:15][CH2:14][C:11]1([N:10]([CH3:19])[C:8](=[O:9])[O:7][C:3]([CH3:4])([CH3:6])[CH3:5])[CH2:12][CH2:13]1

참가 물질

6

반응물 4

HCID 962WaterHCID 10340Sodium CarbonateHCID 4148881Lithium borohydrideHCID 59620515HCID 59620515, 화합물

생성물 1

HCID 70144159HCID 70144159, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

Over 20 minutes, 20 ml of 2M lithium borohydride in tetrahydrofuran is poured, at 20° C., into a mixture containing 4.86 g of the product obtained in Step 4 and 20 ml of tetrahydrofuran. After stirring for 20 hours at ambient temperature and then for 1 hour at reflux, the mixture is cooled to 5° C. and then hydrolysed using a mixture containing 8 ml of water and 4 ml of 10% aqueous sodium carbonate solution. The aqueous phase is extracted several times with ether. After customary treatment, chromatography of the residue over silica gel (CH2Cl2/tetrahydrofuran: 98/2) allows the expected product to be isolated (liquid).

후처리

  1. temperaturefor 1 hour at reflux
  2. temperaturethe mixture is cooled to 5° C.
  3. extractionThe aqueous phase is extracted several times with ether
  4. customto be isolated (liquid)

출처 및 근거

ORD 기록
ord-f186cfb404d144c694c81fdf8916f790
출처 데이터셋
uspto-grants-2005_09
특허 번호
US06943184B2

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