Hexane → HCID 53661366, 화합물

HRID 1492406노트

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HRID 1492406 반응식
[CH:1]12[CH2:9][CH:5]3[CH2:6][CH:7]([CH2:8]1)[C:3]([NH:10][C:11]([C:13]1[CH:18]=[CH:17][N:16]=[CH:15][C:14]=1[CH:19]([C:28]1[CH:33]=[CH:32][C:31]([O:34]C)=[CH:30][CH:29]=1)[C:20]1[CH:25]=[CH:24][C:23]([O:26]C)=[CH:22][CH:21]=1)=[O:12])([CH2:4]3)[CH2:2]2.CCCCCC.B(Br)(Br)Br.C(=O)(O)[O-].[Na+]>C(Cl)Cl>[CH:1]12[CH2:9][CH:5]3[CH2:6][CH:7]([CH2:8]1)[C:3]([NH:10][C:11]([C:13]1[CH:18]=[CH:17][N:16]=[CH:15][C:14]=1[CH:19]([C:28]1[CH:33]=[CH:32][C:31]([OH:34])=[CH:30][CH:29]=1)[C:20]1[CH:25]=[CH:24][C:23]([OH:26])=[CH:22][CH:21]=1)=[O:12])([CH2:4]3)[CH2:2]2

참가 물질

6

반응물 4

HCID 8058HexaneHCID 25134Boron tribromideHCID 516892Sodium BicarbonateHCID 53910045HCID 53910045, 화합물

생성물 1

HCID 53661366HCID 53661366, 화합물수율 26.8%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

In 40 ml of methylene chloride was dissolved 2.5 g of Compound 1 obtained in Example 1, and the solution was cooled to from -5° to -15° C. Then, 20 ml of a hexane solution containing 1M boron tribromide was added thereto. The mixture was stirred at room temperature for two hours and thirty minutes. The reaction mixture was poured into a saturated aqueous sodium bicarbonate solution, followed by extraction with ethyl acetate. The extract was dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography to give 0.63 g of the desired compound as a solid.

후처리

  1. temperaturethe solution was cooled to from -5° to -15° C
  2. additionwas added
  3. extractionfollowed by extraction with ethyl acetate
  4. dry with materialThe extract was dried over anhydrous magnesium sulfate
  5. customThe solvent was evaporated under reduced pressure
  6. customthe residue was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-741c5afad6f54f8b988a6852f4d989f4
출처 데이터셋
uspto-grants-1994_12
특허 번호
US05374634

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