Dimethyl Sulfate → HCID 15341833, 화합물

HRID 893473노트

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HRID 893473 반응식
[NH2:1][C:2]([C:4]1[CH:30]=[CH:29][C:7]([O:8][CH2:9][CH2:10][CH2:11][O:12][C:13]2[C:14]([CH2:26][CH2:27][CH3:28])=[C:15]([CH:23]=[CH:24][CH:25]=2)[O:16][CH2:17][C:18]([O:20][CH2:21][CH3:22])=[O:19])=[C:6]([CH2:31][CH:32]=[CH2:33])[C:5]=1[OH:34])=[O:3].[OH-].[K+].S(OC)(O[CH3:41])(=O)=O.C1COCC1>C(OCC)(=O)C.CCCCCC.O>[NH2:1][C:2]([C:4]1[CH:30]=[CH:29][C:7]([O:8][CH2:9][CH2:10][CH2:11][O:12][C:13]2[C:14]([CH2:26][CH2:27][CH3:28])=[C:15]([CH:23]=[CH:24][CH:25]=2)[O:16][CH2:17][C:18]([O:20][CH2:21][CH3:22])=[O:19])=[C:6]([CH2:31][CH:32]=[CH2:33])[C:5]=1[O:34][CH3:41])=[O:3]

참가 물질

7

반응물 4

HCID 6497Dimethyl SulfateHCID 8028TetrahydrofuranHCID 14797Potassium HydroxideHCID 15341832HCID 15341832, 화합물

생성물 1

HCID 15341833HCID 15341833, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 21226206Ethyl acetate hexane용매

실험 절차

The compound of Example 54 (132 mg, 0.280 mmol), potassium hydroxide (18.8 mg, 0.336 mmol) and dimethyl sulfate (52.9 mg, 0.420 mmol) were added to THF, and the reaction mixture was stirred overnight at room temperature, then 10 ml of water was added, and the layers were separated. The aqueous layer was extracted three times with ethyl acetate, and the combined organic fractions were dried and filtered. The solvent was removed under vacuum to give an oil. Chromatography of the oil on silica gel with 50/50 ethyl acetate/hexane gave the product as a white solid.

후처리

  1. customthe layers were separated
  2. extractionThe aqueous layer was extracted three times with ethyl acetate
  3. customthe combined organic fractions were dried
  4. filtrationfiltered
  5. customThe solvent was removed under vacuum
  6. customto give an oil

출처 및 근거

ORD 기록
ord-fc71d34dedf747e6b5fa718b285610f5
출처 데이터셋
uspto-grants-1992_06
특허 번호
US05124350

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