Hydrochloric Acid → HCID 9816245, 화합물

HRID 586792노트

반응식

HRID 586792 반응식
[CH3:1][Si](C=[N+]=[N-])(C)C.CCCCCC.[OH:14][CH2:15][C:16]([NH:19][C:20](=[O:29])[C:21]1[CH:26]=[CH:25][C:24]([F:27])=[CH:23][C:22]=1[F:28])([CH3:18])[CH3:17].B(F)(F)F.CCOCC.Cl>C(Cl)Cl>[CH3:1][O:14][CH2:15][C:16]([NH:19][C:20](=[O:29])[C:21]1[CH:26]=[CH:25][C:24]([F:27])=[CH:23][C:22]=1[F:28])([CH3:18])[CH3:17]

참가 물질

7

반응물 5

HCID 313Hydrochloric AcidHCID 8000Boron trifluoride etherateHCID 8058HexaneHCID 167693TrimethylsilyldiazomethaneHCID 98374972,4-Difluoro-N-(2-hydroxy-1,1-dimethylethyl)benzamide

생성물 1

HCID 9816245HCID 9816245, 화합물수율 60%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A solution of 2M trimethylsilyldiazomethane in hexane (3.9 ml, 7.8 mmol) was added dropwise to a solution of N-(2-hydroxy-1,1-dimethylethyl)-2,4-difluorobenzamide obtained in Example 27 (0.59 g, 2.6 mmol) and boron trifluoride diethyl etherate (43 mg, 0.3 mmol) in methylene chloride (6 ml), and stirred at room temperature overnight. To the reaction mixture was added 1N hydrochloric acid (5 ml) dropwise, and the resulting mixture was concentrated and extracted with ethyl acetate. The extract was washed with brine, dried over MgSO4 and concentrated under a reduced pressure. The residue was purified by silica gel column chromatography (hexane/ethyl acetate=10/1) to give the title compound (0.38 g; 60%).

후처리

  1. concentrationthe resulting mixture was concentrated
  2. extractionextracted with ethyl acetate
  3. washThe extract was washed with brine
  4. dry with materialdried over MgSO4
  5. concentrationconcentrated under a reduced pressure
  6. customThe residue was purified by silica gel column chromatography (hexane/ethyl acetate=10/1)

출처 및 근거

ORD 기록
ord-413f782ed76844fab623d71d3329d40d
출처 데이터셋
uspto-grants-2005_08
특허 번호
US06936736B2

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