HCID 86756334、化合物 → Sampatrilat

HRID 567943ノート

反応式

HRID 567943 の反応式
O.[C:2]([C@H:5]([CH2:27][NH:28][C:29](=[O:41])[C@H:30]([CH2:36][CH2:37][CH2:38][CH2:39][NH2:40])[NH:31][S:32]([CH3:35])(=[O:34])=[O:33])[CH2:6][C:7]1([C:12]([NH:14][C@H:15]([C:24]([OH:26])=[O:25])[CH2:16][C:17]2[CH:22]=[CH:21][C:20]([OH:23])=[CH:19][CH:18]=2)=[O:13])[CH2:11][CH2:10][CH2:9][CH2:8]1)([OH:4])=[O:3]>O.CC(C)=O>[C:2]([C@H:5]([CH2:27][NH:28][C:29](=[O:41])[C@H:30]([CH2:36][CH2:37][CH2:38][CH2:39][NH2:40])[NH:31][S:32]([CH3:35])(=[O:34])=[O:33])[CH2:6][C:7]1([C:12]([NH:14][C@H:15]([C:24]([OH:26])=[O:25])[CH2:16][C:17]2[CH:22]=[CH:21][C:20]([OH:23])=[CH:19][CH:18]=2)=[O:13])[CH2:11][CH2:10][CH2:9][CH2:8]1)([OH:4])=[O:3]

参加物

4

反応物 1

HCID 86756334HCID 86756334、化合物

生成物 1

HCID 6324648Sampatrilat

試薬・触媒・溶媒 2

HCID 180Acetone溶媒2 回HCID 962Water溶媒

実験手順

(S,S,S)-N-(1-[2-Carboxy-3-(N2-mesyllysylamino)propyl]-1-cyclopentylcarbonyl)tyrosine hydrate (the δ-form, see Preparation 2) (847.0 g) was dissolved in water (762 ml) and the solution diluted with acetone (1.0 l). This solution was added slowly to vigorously stirred acetone (18.05 l) at room temperature and a white solid precipitated. The mixture was stirred at room temperature for 18 hours, the solid was collected by filtration, washed with acetone and dried to give the title compound as a white solid (775 g), m.p. 179-181° C. Found: C,53.42; H,6.88; N,9.37; S,5.49. C26H40N4O9S requires: C,53.41; H,6.90; N,9.58; S,5.48%.

後処理

  1. customPreparation 2) (847.0 g)
  2. customa white solid precipitated
  3. filtrationthe solid was collected by filtration
  4. washwashed with acetone
  5. customdried

出典と根拠

ORDレコード
ord-2d8a21e2f32e4ae68eb74d02fae69bf1
出典データセット
uspto-grants-2001_01
特許番号
US06180665B2

反応ノート

読み込み中…