4H-Pyrido(2,1-a)phthalazine-1-carboxamide, 10-chloro-N,N-diethyl-4-oxo-3-phenyl- → HCID 53647567、化合物

HRID 477806ノート

反応式

HRID 477806 の反応式
[Cl:1][C:2]1[CH:11]=[C:10]2[C:5]([CH:6]=[N:7][N:8]3[C:15](=[O:16])[C:14]([C:17]4[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=4)=[CH:13][C:12]([C:23]([N:25]([CH2:28][CH3:29])[CH2:26][CH3:27])=[O:24])=[C:9]32)=[CH:4][CH:3]=1.[BH4-].[Li+]>O1CCCC1>[Cl:1][C:2]1[CH:11]=[C:10]2[C:5]([CH2:6][NH:7][N:8]3[C:15](=[O:16])[C:14]([C:17]4[CH:18]=[CH:19][CH:20]=[CH:21][CH:22]=4)=[CH:13][C:12]([C:23]([N:25]([CH2:28][CH3:29])[CH2:26][CH3:27])=[O:24])=[C:9]32)=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 30666894H-Pyrido(2,1-a)phthalazine-1-carboxamide, 10-chloro-N,N-diethyl-4-oxo-3-phenyl-HCID 4148881Lithium borohydride2 回

生成物 1

HCID 53647567HCID 53647567、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

2.7 g of 10-chloro-N,N-diethyl-4-oxo-3-phenyl-4H-pyrido[2,1-a]phthalazine-1-carboxamide are suspended in 65 ml of tetrahydrofuran under argon, whereupon 150 mg of lithium borohydride are added thereto, the mixture is stirred at room temperature for 4 hours, an additional 75 mg of lithium borohydride are added thereto and the mixture is stirred further until the reaction finishes. The reaction mixture is poured into 300 ml of ice-water, whereby the product crystallizes out. The crude product is chromatographed on silica gel. By recrystallization from toluene, there is obtained 10-chloro-N,N-diethyl-6,7-dihydro-4-oxo-3-phenyl-4H-pyrido[2,1-a]phthalazine-1-carboxamide of m.p. 192°-194° (toluene).

後処理

  1. additionare added
  2. stirringthe mixture is stirred further until the reaction
  3. customcrystallizes out
  4. customThe crude product is chromatographed on silica gel
  5. customBy recrystallization from toluene

出典と根拠

ORDレコード
ord-b9a40d64ddf54b1d9783742b6953f9e7
出典データセット
uspto-grants-1989_12
特許番号
US04889854

反応ノート

読み込み中…