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Potassium Carbonate → HCID 131716391, 화합물

HRID 1651555
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HRID 1651555 반응식
[C:1]1([CH:7]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)N2CCNCC2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.Cl[CH2:21][CH2:22][S:23][C:24]1[S:25][C:26]2[CH:32]=[CH:31][CH:30]=[CH:29][C:27]=2[N:28]=1.O1[CH2:38][CH2:37]OCC1.C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[C:14]1([CH:7]([C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)[CH:38]2[CH2:37][CH2:24][N:28]([CH2:21][CH2:22][S:23][C:24]3[S:25][C:26]4[CH:32]=[CH:31][CH:30]=[CH:29][C:27]=4[N:28]=3)[CH2:27][CH2:26]2)[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 11430Potassium CarbonateHCID 312751,4-DioxaneHCID 70048BenzhydrylpiperazineHCID 150558582-[(2-Chloroethyl)sulfanyl]-1,3-benzothiazole

생성물 1

HCID 131716391HCID 131716391, 화합물수율 35%

시약·촉매·용매 1

HCID 6228Dimethylformamide
용매

실험 절차

To a mixture of 1.00 g (3.96 mmol) of 4-(diphenylmethyl)-piperazine and 1.28 g (5.57 mmol) of 2-(2-chloroethylthio)benzothiazole, were added 10 ml of dioxane, 2 ml of dimethylformamide and 0.85 g (6.15 mmol) of potassium carbonate, and the mixture was stirred under reflux for 3 hours. After the reaction, the insolubles were filtered off, and the filtrate was concentrated. The residue was separated by silica gel column chromatography using a mixture of chloroform and methanol in the volume ratio 30:1 as the developing solvent, and the desired fraction was concentrated under reduced pressure to give 0.61 g (35%) of 2-[2-[4-(diphenylmethyl)-1-piperadinyl]-ethylthio]benzothiazole as an oil.

후처리

  1. temperatureunder reflux for 3 hours
  2. customAfter the reaction
  3. filtrationthe insolubles were filtered off
  4. concentrationthe filtrate was concentrated
  5. customThe residue was separated by silica gel column chromatography
  6. additiona mixture of chloroform and methanol in the volume ratio 30:1 as the developing solvent
  7. concentrationthe desired fraction was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-be12788ba41d40889f3f284a10adc7b2
출처 데이터셋
uspto-grants-1990_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04929618

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