Methyl 3-aminocrotonate → Phthalimidoamlodipine

HRID 25475

反応式

HRID 25475 の反応式
[Cl:1][C:2]1[CH:31]=[CH:30][CH:29]=[CH:28][C:3]=1[CH:4]=[C:5]([C:11]([CH2:13][O:14][CH2:15][CH2:16][N:17]1[C:21](=[O:22])[C:20]2=[CH:23][CH:24]=[CH:25][CH:26]=[C:19]2[C:18]1=[O:27])=O)[C:6]([O:8][CH2:9][CH3:10])=[O:7].[CH3:32][O:33][C:34](=[O:39])/[CH:35]=[C:36](\[NH2:38])/[CH3:37]>CC(O)C>[Cl:1][C:2]1[CH:31]=[CH:30][CH:29]=[CH:28][C:3]=1[CH:4]1[C:35]([C:34]([O:33][CH3:32])=[O:39])=[C:36]([CH3:37])[NH:38][C:11]([CH2:13][O:14][CH2:15][CH2:16][N:17]2[C:21](=[O:22])[C:20]3[C:19](=[CH:26][CH:25]=[CH:24][CH:23]=3)[C:18]2=[O:27])=[C:5]1[C:6]([O:8][CH2:9][CH3:10])=[O:7]

参加物

4

反応物 2

HCID 643918Methyl 3-aminocrotonateHCID 53879087Ethyl 2-(2-chlorobenzylidene)-4-(2-(1,3-dioxoisoindolin-2-yl)ethoxy)-3-oxobutanoate

生成物 1

HCID 9871958Phthalimidoamlodipine

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

反応条件

温度
15 °C

実験手順

350 g of crude ethyl 2-(o-chlorobenzylidene)-4-(2-phthalimidoethoxy) acetoacetate from Example 1 was dissolved in 540 ml of 2-propanol at 80° C. 50 g of methyl-3-aminocrotonate was added and the mixture was heated at the same temperature for 16 hours. The mixture was evaporated to dryness. The residue was dissolved in 540 ml of glacial acetic acid at 80° C. The mixture was cooled to 15° C. and stirred at the same temperature for 20 hours. The formed solid was filtered off and washed with 280 ml of glacial acetic acid. The solid was suspended in 225 ml of methanol and agitated for 30 minutes. The solid was filtered off, washed with 75 ml of methanol and dried.

後処理

  1. temperaturethe mixture was heated at the same temperature for 16 hours
  2. customThe mixture was evaporated to dryness
  3. dissolutionThe residue was dissolved in 540 ml of glacial acetic acid at 80° C
  4. filtrationThe formed solid was filtered off
  5. washwashed with 280 ml of glacial acetic acid
  6. stirringagitated for 30 minutes
  7. filtrationThe solid was filtered off
  8. washwashed with 75 ml of methanol
  9. customdried

出典と根拠

ORDレコード
ord-373b8316f2424a3bbbfd26a259af20b1
出典データセット
uspto-grants-2005_02
特許番号
US06858738B2

関連ノート

読み込み中…