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Dimethylformamide dimethyl acetal → 6-Dimethylaminomethylene-4,4-diphenylcyclohex-2-enone

HRID 1243853
ノート
印刷プレビュー

反応式

HRID 1243853 の反応式
CO[CH:3](OC)[N:4]([CH3:6])[CH3:5].[C:9]1([C:15]2([C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=3)[CH2:20][CH2:19][C:18](=[O:21])[CH:17]=[CH:16]2)[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1>CN(C)C=O>[CH3:6][N:4]([CH:3]=[C:19]1[C:18](=[O:21])[CH:17]=[CH:16][C:15]([C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)([C:9]2[CH:10]=[CH:11][CH:12]=[CH:13][CH:14]=2)[CH2:20]1)[CH3:5]
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

4

反応物 2

HCID 78373Dimethylformamide dimethyl acetalHCID 1382802-Cyclohexen-1-one, 4,4-diphenyl-

生成物 1

HCID 695944896-Dimethylaminomethylene-4,4-diphenylcyclohex-2-enone収率 56.1%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
20 °C

実験手順

4.77 g of N,N-dimethylformamide dimethyl acetal are added to a solution of 2.48 g of 4,4-diphenylcyclohex-2-enone in 20 Cm3 of N,N-dimethylformamide. The mixture is refluxed for about 4 hours. After cooling to a temperature in the region of 20° C., the solution is concentrated to dryness under reduced pressure (13 kPa). The residue is taken up in 50 cm3 of diisopropyl ether and allowed to precipitate for about 20 hours at a temperature in the region of 20° C. The solid is drained by suction, washed with three times 10 cm3 of diisopropyl ether and then dried under reduced pressure (13 kPa) over potassium hydroxide at a temperature in the region of 20° C. 1.7 g of 6-dimethylaminomethylene-4,4-diphenylcyclohex-2-enone are thus obtained in the form of a cream-coloured powder, the characteristics of which are as follows:

後処理

  1. temperatureThe mixture is refluxed for about 4 hours
  2. concentrationthe solution is concentrated to dryness under reduced pressure (13 kPa)
  3. customto precipitate for about 20 hours at a temperature in the region of 20° C
  4. washwashed with three times 10 cm3 of diisopropyl ether
  5. dry with materialdried under reduced pressure (13 kPa) over potassium hydroxide at a temperature in the region of 20° C

出典と根拠

ORDレコード
ord-f10d5c490f904ada9c2731611ed62f1a
出典データセット
uspto-grants-2006_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07119115B2

反応ノート

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