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Triethylamine → HCID 14371864、化合物

HRID 1381948
ノート
印刷プレビュー

反応式

HRID 1381948 の反応式
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]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 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、化合物

生成物 1

HCID 14371864HCID 14371864、化合物収率 67.6%

試薬・触媒・溶媒 2

HCID 962Water溶媒
HCID 6228Dimethylformamide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-b4b02d44d4b444d9839357b00232371c
出典データセット
uspto-grants-1989_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04804665

反応ノート

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