Sodium Hydroxide → Regadenoson Impurity 1

HRID 2168567

反応式

HRID 2168567 の反応式
[OH:1][C@@H:2]1[C@H:6]([OH:7])[C@@H:5]([CH2:8][OH:9])[O:4][C@H:3]1[N:10]1[CH:18]=[N:17][C:16]2[C:11]1=[N:12][C:13]([N:20]1[CH:24]=[C:23]([C:25]([O:27]CC)=[O:26])[CH:22]=[N:21]1)=[N:14][C:15]=2[NH2:19].[OH-].[Na+]>>[OH:1][C@@H:2]1[C@H:6]([OH:7])[C@@H:5]([CH2:8][OH:9])[O:4][C@H:3]1[N:10]1[CH:18]=[N:17][C:16]2[C:11]1=[N:12][C:13]([N:20]1[CH:24]=[C:23]([C:25]([OH:27])=[O:26])[CH:22]=[N:21]1)=[N:14][C:15]=2[NH2:19]

参加物

3

反応物 2

HCID 14798Sodium HydroxideHCID 9865974Ethyl 1-(6-amino-9-((2R,3R,4S,5R)-3,4-dihydroxy-5-(hydroxymethyl)tetrahydrofuran-2-yl)-9H-purin-2-yl)-1H-pyrazole-4-carboxylate

生成物 1

HCID 9864495Regadenoson Impurity 1

実験手順

Compound 12 (0.05 mg, 0.12 mmol) was dissolved one equivalent of 1N NaOH. The solution was allowed to stir at Rt for 2 h, then acidified to pH 4. The resulting precipitate was filtered and washed with water and ether. 1HNMR (CD3OD) δ 3.75 (m, 1 H), 3.90 (m, 1 H), 4.13 (d, 1 H), 4.43 (d, 1 H), 4.64 (m, 1 H), 6.05 (d, 1 H), 8.10 (s, 1 H), 8.35 (s, 1 H), 9.05 (s, 1 H).

後処理

  1. filtrationThe resulting precipitate was filtered
  2. washwashed with water and ether

出典と根拠

ORDレコード
ord-264d8f982b974933ae76aa30406ac7d5
出典データセット
uspto-grants-2015_06
特許番号
US09045519B2

関連ノート

読み込み中…