Dimethyl Sulfate → HCID 53758088, 화합물

HRID 1756200노트

반응식

HRID 1756200 반응식
[CH3:1][O:2][C:3]([C:5]1(CCC)[CH2:10][CH2:9][C:8]2[CH:11]=[CH:12][C:13]([O:15][CH2:16][CH2:17][CH2:18][O:19][C:20]3[CH:25]=[CH:24][C:23]([C:26]([N:28]4[CH2:32][CH2:31][CH2:30][CH2:29]4)=[O:27])=[C:22]([OH:33])[C:21]=3[CH2:34][CH:35]=[CH2:36])=[CH:14][C:7]=2[O:6]1)=[O:4].S(OC)(O[CH3:44])(=O)=O.[OH-].[K+]>C1COCC1>[CH3:44][O:33][C:22]1[C:21]([CH2:34][CH:35]=[CH2:36])=[C:20]([CH:25]=[CH:24][C:23]=1[C:26]([N:28]1[CH2:32][CH2:31][CH2:30][CH2:29]1)=[O:27])[O:19][CH2:18][CH2:17][CH2:16][O:15][C:13]1[CH:12]=[CH:11][C:8]2[CH2:9][CH2:10][CH:5]([C:3]([O:2][CH3:1])=[O:4])[O:6][C:7]=2[CH:14]=1

참가 물질

5

반응물 3

HCID 6497Dimethyl SulfateHCID 14797Potassium HydroxideHCID 19917189HCID 19917189, 화합물

생성물 1

HCID 53758088HCID 53758088, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

The compound of Example 27 (280 mg, 0.51 mmol) dimethyl sulfate (192 mg, 153 mmol) and potassium hydroxide (57 mg, 1 mmol) was added to about 20 ml of THF, and the reaction mixture was stirred overnight at room temperature. The reaction mixture was washed with water and thoroughly extracted with ethyl acetate. The organic layer was dried over magnesium sulfate and concentrated in vacuo. Chromatography of the crude material on silica gel using 75% ethyl acetate/hexane as eluant gave the product.

후처리

  1. washThe reaction mixture was washed with water
  2. extractionthoroughly extracted with ethyl acetate
  3. dry with materialThe organic layer was dried over magnesium sulfate
  4. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-865f2e2570344361b0c45517448ea7be
출처 데이터셋
uspto-grants-1995_08
특허 번호
US05439937

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