Monosodium Citrate → Tofacitinib Citrate

HRID 1775142

反応式

HRID 1775142 の反応式
[CH3:1][C@H:2]1[C@@H:7]([N:8]([C:10]2[N:18]=[CH:17][N:16]=[C:15]3[C:11]=2[CH:12]=[CH:13][NH:14]3)[CH3:9])[CH2:6][N:5]([C:19]([CH2:21][C:22]#[N:23])=[O:20])[CH2:4][CH2:3]1.Br.[C:25]([O-:37])(=[O:36])[CH2:26][C:27]([CH2:32][C:33]([OH:35])=[O:34])([C:29]([OH:31])=[O:30])[OH:28].[Na+]>O>[CH3:1][C@H:2]1[C@@H:7]([N:8]([C:10]2[N:18]=[CH:17][N:16]=[C:15]3[C:11]=2[CH:12]=[CH:13][NH:14]3)[CH3:9])[CH2:6][N:5]([C:19]([CH2:21][C:22]#[N:23])=[O:20])[CH2:4][CH2:3]1.[CH2:32]([C:27]([OH:28])([C:29]([OH:31])=[O:30])[CH2:26][C:25]([OH:37])=[O:36])[C:33]([OH:35])=[O:34]

参加物

4

反応物 2

HCID 23666341Monosodium CitrateHCID 131734730HCID 131734730、化合物

生成物 1

HCID 10174505Tofacitinib Citrate収率 89.3%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
25 °C

実験手順

Amorphous tofacitinib hydrobromide (0.55 g) was dissolved in water (6 mL). The solution was treated with solid monosodium citrate (0.40 g, 1.69 mmol) and the resulting white suspension was stirred for 16 hours at 25° C. The suspension was filtered, washed with water (2×5 mL) and air-dried for 16 hours at 25° C. to yield 0.63 g of tofacitinib citrate as a white solid.

後処理

  1. filtrationThe suspension was filtered
  2. washwashed with water (2×5 mL)
  3. customair-dried for 16 hours at 25° C.

出典と根拠

ORDレコード
ord-749e280bbddb45d38834f9f5890e8c66
出典データセット
uspto-grants-2016_02
特許番号
US09260438B2

関連ノート

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