Hydrochloric Acid → Methyl deoxycholate

HRID 586111

反応式

HRID 586111 の反応式
[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]

参加物

4

反応物 3

HCID 313Hydrochloric AcidHCID 887MethanolHCID 222528Deoxycholic Acid

生成物 1

HCID 229346Methyl deoxycholate収率 92%

実験手順

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:

後処理

  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

出典と根拠

ORDレコード
ord-1cca3e62b96c4d18a79d5b887c7271b8
出典データセット
uspto-grants-2005_08
特許番号
US06936402B2

関連ノート

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