Ethanol → Methyldigoxin

HRID 973379

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HRID 973379 반응식
[CH3:1][C@H:2]1[O:7][C@@H:6]([O:8][C@H:9]2[C@@H:14]([OH:15])[CH2:13][C@H:12]([O:16][C@H:17]3[C@@H:22]([OH:23])[CH2:21][C@H:20]([O:24][C@@H:25]4[CH2:30][C@H:29]5[CH2:31][CH2:32][C@H:33]6[C@@:38]7([OH:48])[CH2:39][CH2:40][C@H:41]([C:42]8[CH2:47][O:46][C:44](=[O:45])[CH:43]=8)[C@@:37]7([CH3:49])[C@H:36]([OH:50])[CH2:35][C@@H:34]6[C@@:28]5([CH3:51])[CH2:27][CH2:26]4)[O:19][C@@H:18]3[CH3:52])[O:11][C@@H:10]2[CH3:53])[CH2:5][C@H:4]([OH:54])[C@@H:3]1[OH:55].[CH2:56](O)C>>[CH3:1][C@H:2]1[O:7][C@@H:6]([O:8][C@H:9]2[C@@H:14]([OH:15])[CH2:13][C@H:12]([O:16][C@H:17]3[C@@H:22]([OH:23])[CH2:21][C@H:20]([O:24][C@@H:25]4[CH2:30][C@H:29]5[CH2:31][CH2:32][C@H:33]6[C@@:38]7([OH:48])[CH2:39][CH2:40][C@H:41]([C:42]8[CH2:47][O:46][C:44](=[O:45])[CH:43]=8)[C@@:37]7([CH3:49])[C@H:36]([OH:50])[CH2:35][C@@H:34]6[C@@:28]5([CH3:51])[CH2:27][CH2:26]4)[O:19][C@@H:18]3[CH3:52])[O:11][C@@H:10]2[CH3:53])[CH2:5][C@H:4]([OH:54])[C@@H:3]1[O:55][CH3:56]

참가 물질

3

반응물 2

HCID 702EthanolHCID 2724385Digoxin

생성물 1

HCID 443946Methyldigoxin

실험 절차

4.75 l. of eluate with 40% ethanol contain 3.91 g. of solid material. The mixture contains all non-reacted digoxin, α-metildigoxin and β-metildigoxin and can again be separated on the column. The following fraction of 5 l. contains 4.73 g. of slightly contaminated β-metildigoxin. If the ethanol content is increased, diethers and higher ethers of digoxin are eluted. The main fraction with metildigoxin is reprecipitated from methanol/water, boiled up with chloroform and stirred up with acetone.

후처리

  1. customcan again be separated on the column
  2. temperatureIf the ethanol content is increased
  3. washdiethers and higher ethers of digoxin are eluted
  4. customThe main fraction with metildigoxin is reprecipitated from methanol/water

출처 및 근거

ORD 기록
ord-075096f1ce5b48c6bbe6b30e253ce676
출처 데이터셋
uspto-grants-1991_11
특허 번호
US05062959

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