Hydrochloric Acid → Methyl deoxycholate

HRID 586111

반응식

HRID 586111 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].Cl.[CH3:30]O>>[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][CH3:30])=[O:6]

참가 물질

4

반응물 3

HCID 313Hydrochloric AcidHCID 887MethanolHCID 222528Deoxycholic Acid

생성물 1

HCID 229346Methyl deoxycholate수율 92%

실험 절차

100 g of deoxycholic acid was dissolved in 300 ml of methanol, and then 2 ml of hydrochloric acid was added thereto. The resulting mixture was refluxed for 1 hour. The methanol was distilled off. After the resulting mixture was dissolved in 400 ml of ethylether, it was washed with distilled water, sodium bicarbonate and brine several times. The separated organic layer was dried over anhydrous magnesium sulfate, concentrated and dried in vacuo to prepare 95 g (yield: 92%) of methyl deoxycholate represented by the following formula:

후처리

  1. temperatureThe resulting mixture was refluxed for 1 hour
  2. distillationThe methanol was distilled off
  3. dissolutionAfter the resulting mixture was dissolved in 400 ml of ethylether
  4. washit was washed with distilled water, sodium bicarbonate and brine several times
  5. dry with materialThe separated organic layer was dried over anhydrous magnesium sulfate
  6. concentrationconcentrated
  7. customdried in vacuo

출처 및 근거

ORD 기록
ord-1cca3e62b96c4d18a79d5b887c7271b8
출처 데이터셋
uspto-grants-2005_08
특허 번호
US06936402B2

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