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Potassium Carbonate → HCID 131716391、化合物

HRID 1651555
ノート
印刷プレビュー

反応式

HRID 1651555 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

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

生成物 1

HCID 131716391HCID 131716391、化合物収率 35%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide
溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-be12788ba41d40889f3f284a10adc7b2
出典データセット
uspto-grants-1990_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04929618

反応ノート

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