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Triethylamine → HCID 14371864, 화합물

HRID 1381948
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HRID 1381948 반응식
Cl.[CH3:2][O:3][N:4]1[C:8](=[O:9])[CH2:7][C:6]2([CH2:14][CH2:13][NH:12][CH2:11][CH2:10]2)[C:5]1=[O:15].[CH3:16][C:17]1[NH:18][C:19]([CH3:39])=[C:20]([C:35]([O:37][CH3:38])=[O:36])[CH:21]([C:26]2[CH:31]=[CH:30][CH:29]=[C:28]([N+:32]([O-:34])=[O:33])[CH:27]=2)[C:22]=1[C:23](O)=[O:24].C(N(CC)CC)C.P(OC#N)(OCC)(OCC)=O>CN(C)C=O.O>[CH3:16][C:17]1[NH:18][C:19]([CH3:39])=[C:20]([C:35]([O:37][CH3:38])=[O:36])[CH:21]([C:26]2[CH:31]=[CH:30][CH:29]=[C:28]([N+:32]([O-:34])=[O:33])[CH:27]=2)[C:22]=1[C:23]([N:12]1[CH2:13][CH2:14][C:6]2([C:5](=[O:15])[N:4]([O:3][CH3:2])[C:8](=[O:9])[CH2:7]2)[CH2:10][CH2:11]1)=[O:24]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 8471TriethylamineHCID 1733222,6-Dimethyl-4-(3-nitrophenyl)-1,4-dihydropyridine-3,5-dicarboxylic acid monomethyl esterHCID 30882852,8-Diazaspiro(4,5)decane-1,3-dione, 2-methoxy-, monohydrochlorideHCID 18315342HCID 18315342, 화합물

생성물 1

HCID 14371864HCID 14371864, 화합물수율 67.6%

시약·촉매·용매 2

HCID 962Water용매
HCID 6228Dimethylformamide용매

실험 절차

To a solution of of 2-methoxy-2,8-diazaspiro[4,5]decane-1,3-dione.hydrochloride (0.21 g) obtained in Example 9, 1,4-dihydro-2,6-dimethyl-5-methoxycarbonyl-4-(3-nitrophenyl)pyridine-3-carboxylic acid (0.3 g) and triethylamine (0.26 ml) in dimethylformamide (7 ml) was added dropwise, under ice-cooling, 0.22 ml of diethyl cyano phosphate, and the mixture was stirred for 30 minutes. To the reaction mixture was added water (20 ml), which was stirred at room temperature, followed by extraction with dichloromethane. The dichloromethane solution was dried over anhydrous sodium sulfate. The solvent was then evaporated off under reduced pressure. The residual oily product was subjected to a silica gel column chromatography (eluent, ethyl acetate), and the solvent for the solution containing the desired product was evaporated off under reduced pressure. The residual solid was recrystallized from ethanol to obtain 0.31 g of yellow crystals, m.p. 228° to 230° C.

후처리

  1. temperaturecooling
  2. extractionfollowed by extraction with dichloromethane
  3. dry with materialThe dichloromethane solution was dried over anhydrous sodium sulfate
  4. customThe solvent was then evaporated off under reduced pressure
  5. additionthe solvent for the solution containing the desired product
  6. customwas evaporated off under reduced pressure
  7. customThe residual solid was recrystallized from ethanol

출처 및 근거

ORD 기록
ord-b4b02d44d4b444d9839357b00232371c
출처 데이터셋
uspto-grants-1989_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04804665

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