Hydrochloric Acid → Gemcitabine Hydrochloride

HRID 217107

반응식

HRID 217107 반응식
[CH:1]1[C:7]([NH2:8])=[N:6][C:4](=[O:5])[N:3]([C@@H:9]2[O:13][C@H:12]([CH2:14][OH:15])[C@@H:11]([OH:16])[C:10]2([F:18])[F:17])[CH:2]=1.[ClH:19]>C(COC)OC>[CH:1]1[C:7]([NH2:8])=[N:6][C:4](=[O:5])[N:3]([C@@H:9]2[O:13][C@H:12]([CH2:14][OH:15])[C@@H:11]([OH:16])[C:10]2([F:17])[F:18])[CH:2]=1.[ClH:19]

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 60750Gemcitabine

생성물 1

HCID 60749Gemcitabine Hydrochloride

시약·촉매·용매 1

HCID 80711,2-Dimethoxyethane용매

반응 조건

온도
64 °C

실험 절차

To the 20 g of thick oil of Gemcitabine base as obtained in example 3 was added Monoglyme (120 ml) and the mixture was heated at 60-68°C. and stirred for 15 minutes. Conc. HCl (10 ml) was then added to the mixture and the contents were heated at same temperature for one hour. Reaction mass was then cooled to 10-15° C. and maintained for 30 minutes. The solid thus obtained is filtered off and washed with Monoglyme and dried under vacuum at 55-60° C. to get 8 g material having HPLC purity with 85% β-anomer & 9% α-anomer, Specific Optical Rotation i.e.[α]D=+40°

후처리

  1. temperaturethe contents were heated at same temperature for one hour
  2. customReaction mass
  3. temperaturewas then cooled to 10-15° C.
  4. temperaturemaintained for 30 minutes
  5. customThe solid thus obtained
  6. filtrationis filtered off
  7. washwashed with Monoglyme
  8. customdried under vacuum at 55-60° C.

출처 및 근거

ORD 기록
ord-0c980c678b044690a140b96cba6b62f9
출처 데이터셋
uspto-grants-2012_06
특허 번호
US08193354B2

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