Dimethyl methoxymethylenemalonate → HCID 71284791、化合物

HRID 1481681ノート

反応式

HRID 1481681 の反応式
CC([N:5]=[C:6]([C:10]1[CH:11]=[C:12]2[C:17](=[CH:18][CH:19]=1)[N:16]([CH3:20])[CH2:15][CH2:14][CH2:13]2)[CH2:7][CH2:8][CH3:9])(C)C.C[O:22][CH:23]=[C:24]([C:29]([O:31][CH3:32])=[O:30])[C:25](OC)=O>COCCOCCOC>[CH2:8]([C:7]1[CH:25]=[C:24]([C:29]([O:31][CH3:32])=[O:30])[C:23](=[O:22])[NH:5][C:6]=1[C:10]1[CH:11]=[C:12]2[C:17](=[CH:18][CH:19]=1)[N:16]([CH3:20])[CH2:15][CH2:14][CH2:13]2)[CH3:9]

参加物

4

反応物 2

HCID 90770Dimethyl methoxymethylenemalonateHCID 89422940HCID 89422940、化合物

生成物 1

HCID 71284791HCID 71284791、化合物収率 17.1%

試薬・触媒・溶媒 1

HCID 8150Diglyme溶媒

反応条件

温度
160 °C

実験手順

To a suspension of 2-methyl-N-(1-(1-methyl-1,2,3,4-tetrahydroquinolin-6-yl)butylidene)propan-2-amine (1.96 g, ca. 7.2 mmol) in diglyme (7 mL) was added dimethyl 2-(methoxymethylene)malonate (2.12 g, 12.2 mmol, 1.7 eq). The reaction was stirred at 160° C. for 3 h then was cooled to room temperature. The precipitate was collected by filtration then washed with Et2O to afford the title compound (402 mg, ca. 1.23 mmol) which was carried over to next step without further purification.

後処理

  1. temperaturethen was cooled to room temperature
  2. filtrationThe precipitate was collected by filtration
  3. washthen washed with Et2O

出典と根拠

ORDレコード
ord-25bf2ced89464f15b55c79841e0b3abd
出典データセット
uspto-grants-2016_08
特許番号
US09409905B2

反応ノート

読み込み中…