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Hydrochloric Acid → N-(5,6-dihydro-7H-cyclopenta[d]pyrimidin-4-yl)-4-[(1-benzyl-4-piperidinyliden)acetyl]aniline

HRID 976135
ノート
印刷プレビュー

反応式

HRID 976135 の反応式
[CH2:1]([N:8]1[CH2:13][CH2:12][C:11](=[CH:14][C:15]([C:17]2[CH:23]=[CH:22][C:20]([NH2:21])=[CH:19][CH:18]=2)=[O:16])[CH2:10][CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Cl[C:25]1[C:26]2[CH2:33][CH2:32][CH2:31][C:27]=2[N:28]=[CH:29][N:30]=1.Cl.C[O-].[Na+].CO>C(O)C.C(Cl)(Cl)Cl>[N:28]1[C:27]2[CH2:31][CH2:32][CH2:33][C:26]=2[C:25]([NH:21][C:20]2[CH:19]=[CH:18][C:17]([C:15](=[O:16])[CH:14]=[C:11]3[CH2:12][CH2:13][N:8]([CH2:1][C:2]4[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=4)[CH2:9][CH2:10]3)=[CH:23][CH:22]=2)=[N:30][CH:29]=1
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 313Hydrochloric AcidHCID 133124494-chloro-5H,6H,7H-cyclopenta[d]pyrimidineHCID 199689364-[(1-Benzyl-4-piperidinyliden)acetyl]anilineHCID 23694274Sodium methanolate methanol

生成物 1

HCID 19968955N-(5,6-dihydro-7H-cyclopenta[d]pyrimidin-4-yl)-4-[(1-benzyl-4-piperidinyliden)acetyl]aniline収率 9.3%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒2 回
HCID 6212Chloroform溶媒

実験手順

To a mixed solvent of 40 ml of chloroform and 20 ml of ethanol were added 2.33 g of 4-[(1-benzyl-4-piperidinyliden)acetyl]aniline and 1.63 g of 4-chloro-5,6-dihydro-7H-cyclopenta[d]pyrimidine, and further 6 ml of an ethanol solution of hydrochloric acid (containing 0.4 g of hydrochloric acid) was added to the mixture and the mixture was stirred at 50° to 60° C. for 3.5 hours under heating. Then, under ice cooling, a 28% sodium methylate-methanol solution was added to the mixture to make it alkaline, and then the solvent was removed by distillation under reduced pressure and the obtained residue was applied to silica gel column chromatography to obtain 0.3 g of the title compound as yellowish white powder.

後処理

  1. additionwas added to the mixture
  2. temperatureunder heating
  3. customthe solvent was removed by distillation under reduced pressure

出典と根拠

ORDレコード
ord-c604b693fb414f41ba6609961b02d93f
出典データセット
uspto-grants-1997_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05610303

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート