Hydrochloric Acid → Gemcitabine Hydrochloride

HRID 217106

反応式

HRID 217106 の反応式
[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]

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 60750Gemcitabine

生成物 1

HCID 60749Gemcitabine Hydrochloride

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

反応条件

温度
12.5 °C

実験手順

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.

後処理

  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.

出典と根拠

ORDレコード
ord-e4b3723cf41e44089ee9b2568a14a59f
出典データセット
uspto-grants-2012_06
特許番号
US08193354B2

関連ノート

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