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Diisopropylamine → HCID 70069641、化合物

HRID 1067302
ノート
印刷プレビュー

反応式

HRID 1067302 の反応式
[CH:1]([NH:4][CH:5]([CH3:7])C)([CH3:3])C.C([Li])CCC.[CH3:13][O:14][CH2:15][O:16][C:17](=[O:37])[CH2:18]/[C:19](/[C:33]([O:35][CH3:36])=[O:34])=[C:20](/[C:22]1[CH:27]=[C:26]([O:28][CH3:29])[C:25]([O:30][CH3:31])=[C:24]([Cl:32])[CH:23]=1)\[CH3:21].[Cl-].[NH4+].[O:40]1CC[CH2:42][CH2:41]1>CCCCCC>[CH3:13][O:14][CH2:15][O:16][C:17](=[O:37])[CH:18]([CH:41]([C:42]1[CH:3]=[CH:1][N:4]=[CH:5][CH:7]=1)[OH:40])/[C:19](/[C:33]([O:35][CH3:36])=[O:34])=[C:20](/[C:22]1[CH:27]=[C:26]([O:28][CH3:29])[C:25]([O:30][CH3:31])=[C:24]([Cl:32])[CH:23]=1)\[CH3:21]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 5

HCID 7912DiisopropylamineHCID 8028Tetrahydrofuran3 回HCID 25517Ammonium ChlorideHCID 70070414HCID 70070414、化合物HCID 178418339Butyllithium

生成物 1

HCID 70069641HCID 70069641、化合物

試薬・触媒・溶媒 1

HCID 8058
Hexane
溶媒

反応条件

温度
-78 °C

実験手順

To a solution of diisopropylamine (1.33 ml) in tetrahydrofuran (20 ml) is added gradually and dropwise a 1.6 N solution of n-butyl lithium in hexane (5.91 ml) at 0° C., and the mixture is stirred at the same temperature for 30 minutes. The solution is cooled to −78° C., and thereto is added gradually and dropwise a solution of (Z)-4-(3-chloro-4,5-dimethoxyphenyl)-4-methyl-3-methoxycarbonyl-3-butenoic acid methoxymethyl ester (2.94 g) in tetrahydrofuran (20 ml), and the mixture is further stirred at the same temperature for 30 minutes. The reaction mixture is cooled to −90° C., and thereto is added gradually and dropwise a solution of isonictinaldehyde (1.01 g) in tetrahydrofuran (10 ml), and the mixture is stirred at −90° C. for 20 minutes. To the reaction mixture is added a saturated aqueous ammonium chloride solution, and the mixture is extracted with ethyl acetate. The organic layer is washed, dried, and concentrated under reduced pressure to remove the solvent to give (Z)-4-(3-chloro-4,5-dimethoxyphenyl)-4-methyl-3-methoxycarbonyl-2-(4-pyridylhydroxymethyl)-3-butenoic acid methoxymethyl ester.

後処理

  1. additionis added gradually
  2. temperatureThe reaction mixture is cooled to −90° C.
  3. additionis added gradually
  4. extractionthe mixture is extracted with ethyl acetate
  5. washThe organic layer is washed
  6. customdried
  7. concentrationconcentrated under reduced pressure
  8. customto remove the solvent

出典と根拠

ORDレコード
ord-f566a2f0cc034778b0c865b0eb86ee36
出典データセット
uspto-grants-2001_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06248743B1

反応ノート

読み込み中…

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