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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
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HRID 976135 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 133124494-chloro-5H,6H,7H-cyclopenta[d]pyrimidineHCID 199689364-[(1-Benzyl-4-piperidinyliden)acetyl]anilineHCID 23694274Sodium methanolate methanol

생성물 1

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

시약·촉매·용매 2

HCID 702Ethanol용매2회
HCID 6212Chloroform용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-c604b693fb414f41ba6609961b02d93f
출처 데이터셋
uspto-grants-1997_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05610303

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