Methyl iodide → Methyl deoxycholate

HRID 1587020

반응식

HRID 1587020 반응식
[CH3:1][C@@H:2]([C@@H:8]1[C@@:12]2([CH3:28])[C@@H:13]([OH:27])[CH2:14][C@@H:15]3[C@@:20]4([CH3:26])[CH2:21][CH2:22][C@@H:23]([OH:25])[CH2:24][C@H:19]4[CH2:18][CH2:17][C@H:16]3[C@@H:11]2[CH2:10][CH2:9]1)[CH2:3][CH2:4][C:5]([OH:7])=[O:6].[C:29](=O)([O-])[O-].[K+].[K+].CI>CN(C)C=O.C(OCC)(=O)C>[CH3:1][C@@H:2]([C@@H:8]1[C@@:12]2([CH3:28])[C@@H:13]([OH:27])[CH2:14][C@@H:15]3[C@@:20]4([CH3:26])[CH2:21][CH2:22][C@@H:23]([OH:25])[CH2:24][C@H:19]4[CH2:18][CH2:17][C@H:16]3[C@@H:11]2[CH2:10][CH2:9]1)[CH2:3][CH2:4][C:5]([O:7][CH3:29])=[O:6]

참가 물질

6

반응물 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 222528Deoxycholic Acid

생성물 1

HCID 229346Methyl deoxycholate

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

실험 절차

To a mixture of deoxycholic acid (25.0 g) and anhydrous potassium carbonate (8.8 g) in anhydrous dimethylformamide (65 ml) is added methyl iodide (4.8 ml) and the mixture stirred at room temperature for about 4 hours. The mixture is diluted with ethyl acetate and washed four times with water and once with saturated sodium chloride solution. The organic solution is dried over magnesium sulfate, filtered, and concentrated in vacuo. The crude product is purified by flash chromatography in 80% ethyl acetate in hexane to give the desired product.

후처리

  1. washwashed four times with water
  2. dry with materialThe organic solution is dried over magnesium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated in vacuo
  5. customThe crude product is purified by flash chromatography in 80% ethyl acetate in hexane

출처 및 근거

ORD 기록
ord-63bcb149b9b44fbcaceb542a47bf9caf
출처 데이터셋
uspto-grants-1993_06
특허 번호
US05216015

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