Hydrochloric Acid → Gemcitabine Hydrochloride

HRID 217106

반응식

HRID 217106 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]>O1CCOCC1>[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 312751,4-Dioxane용매

반응 조건

온도
12.5 °C

실험 절차

To the 20 g of thick oil of Gemcitabine base obtained as in example 3 was added 1,4-Dioxane (120 ml) and the mixture was heated to 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 was filtered off and washed with 1,4-Dioxane and dried under vacuum at 55-60° C. to get 8 g material with Specific Optical Rotation i.e.[α]D=+40° and HPLC purity of 85% β-anomer and 8% α-anomer.

후처리

  1. temperaturethe mixture was heated to 60°-68° C.
  2. temperaturethe contents were heated at same temperature for one hour
  3. customReaction mass
  4. temperaturemaintained for 30 minutes
  5. customThe solid thus obtained
  6. filtrationwas filtered off
  7. washwashed with 1,4-Dioxane
  8. customdried under vacuum at 55-60° C.

출처 및 근거

ORD 기록
ord-e4b3723cf41e44089ee9b2568a14a59f
출처 데이터셋
uspto-grants-2012_06
특허 번호
US08193354B2

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