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

HRID 477806노트

반응식

HRID 477806 반응식
[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

참가 물질

4

반응물 2

HCID 30666894H-Pyrido(2,1-a)phthalazine-1-carboxamide, 10-chloro-N,N-diethyl-4-oxo-3-phenyl-HCID 4148881Lithium borohydride2회

생성물 1

HCID 53647567HCID 53647567, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-b9a40d64ddf54b1d9783742b6953f9e7
출처 데이터셋
uspto-grants-1989_12
특허 번호
US04889854

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