2-(Methylamino)ethanol → Rifamycin

HRID 1415408

반응식

HRID 1415408 반응식
CNCCO.[CH3:6][C:7]1[C:12]2[O:13][C@:14]3([CH3:54])[O:17][CH:18]=[CH:19][C@H:20]([O:52][CH3:53])[C@@H:21]([CH3:51])[C@@H:22]([O:47][C:48]([CH3:50])=[O:49])[C@H:23]([CH3:46])[C@H:24]([OH:45])[C@H:25]([CH3:44])[C@@H:26]([OH:43])[C@@H:27]([CH3:42])[CH:28]=[CH:29][CH:30]=[C:31]([CH3:41])[C:32]([NH:34][C:35]4[C:39](=[O:40])[C:9](=[C:10]([C:37](=[O:38])[CH:36]=4)[C:11]=2[C:15]3=[O:16])[C:8]=1[OH:55])=[O:33]>O1CCOCC1>[CH3:6][C:7]1[C:12]2[O:13][C@@:14]3([CH3:54])[C:15]([C:11]=2[C:10]2[C:37]([OH:38])=[CH:36][C:35]([NH:34][C:32]([C:31]([CH3:41])=[CH:30][CH:29]=[CH:28][C@H:27]([CH3:42])[C@H:26]([OH:43])[C@@H:25]([CH3:44])[C@@H:24]([OH:45])[C@@H:23]([CH3:46])[C@H:22]([O:47][C:48]([CH3:50])=[O:49])[C@H:21]([CH3:51])[C@@H:20]([O:52][CH3:53])[CH:19]=[CH:18][O:17]3)=[O:33])=[C:39]([OH:40])[C:9]=2[C:8]=1[OH:55])=[O:16]

참가 물질

4

반응물 2

HCID 80162-(Methylamino)ethanolHCID 6436726Rifamycin S

생성물 1

HCID 6324616Rifamycin

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

10 g (0.13 mol) of N-methylethanolamine are added to a solution of 21 g (0.03 mol) of rifamycin-S in 20 ml of dioxan and the whole heated for 15 minutes on a boiling water bath. The batch is then evaporated to dryness in vacuo and the residue chromatographed on 2kg of silica gel, using chloroform as eluant. In addition to a dark-colored head zone, two strong, yellow-colored bands are observed. The eluate of the more slowly eluted band is evaporated and the residue crystallized from aqueous methanol. After three crystallizations from aqueous methanol there is obtained 3-N-methylethanol-amino)-rifamycin-SV in the form of coarse prisms melting at 218° C (with decomposition.

후처리

  1. temperaturethe whole heated for 15 minutes on a boiling water bath
  2. customThe batch is then evaporated to dryness in vacuo
  3. customthe residue chromatographed on 2kg of silica gel
  4. additionIn addition to a dark-colored head zone, two strong
  5. customThe eluate of the more slowly eluted band is evaporated
  6. customthe residue crystallized from aqueous methanol
  7. customAfter three crystallizations from aqueous methanol

출처 및 근거

ORD 기록
ord-c4a699024f8f439d8291345532d8ac06
출처 데이터셋
uspto-grants-1977_01
특허 번호
US04005077

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