Potassium Carbonate → HCID 178482552、化合物

HRID 493698

反応式

HRID 493698 の反応式
[CH3:1][N:2]1[C:6]([CH3:7])=[C:5]([C:8]([OH:10])=O)[S:4]/[C:3]/1=[N:11]\[CH3:12].[Cl:13][C:14]1[CH:15]=[C:16]2[C:21](=[CH:22][CH:23]=1)[CH:20]=[C:19]([S:24]([CH2:27][CH2:28][C:29]([N:31]1[CH2:36][CH2:35][NH:34][CH2:33][CH2:32]1)=[O:30])(=[O:26])=[O:25])[CH:18]=[CH:17]2.C1C=CC2N(O)N=NC=2C=1.CCN=C=NCCCN(C)C.C(=O)([O-])[O-].[K+].[K+]>ClCCl.C(N(CC)CC)C>[Cl:13][C:14]1[CH:15]=[C:16]2[C:21](=[CH:22][CH:23]=1)[CH:20]=[C:19]([S:24]([CH2:27][CH2:28][C:29]([N:31]1[CH2:32][CH2:33][N:34]([C:8]([C:5]3[S:4]/[C:3](=[N:11]\[CH3:12])/[N:2]([CH3:1])[C:6]=3[CH3:7])=[O:10])[CH2:35][CH2:36]1)=[O:30])(=[O:26])=[O:25])[CH:18]=[CH:17]2

参加物

8

反応物 5

HCID 11430Potassium CarbonateHCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 757711-HydroxybenzotriazoleHCID 231308831-(3-((6-Chloro-2-naphthyl)sulfonyl)propionyl)piperazineHCID 178482553HCID 178482553、化合物

生成物 1

HCID 178482552HCID 178482552、化合物収率 8.9%

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 8471Triethylamine溶媒

実験手順

(2Z)-3,4-Dimethyl-2-methylimino-2,3-dihydro-1,3-thiazole-5-carboxylic acid (0.6 g) was dissolved in dichloromethane (30 mL), and triethylamine (0.14 mL) was added thereto. With ice cooling, 1-(3-((6-chloro-2-naphthyl)sulfonyl)propionyl)piperazine (1.0 g), HOBt (0.42 g) and WSC (0.57 g) were added thereto, and the mixture was mixed at room temperature for 16 hours. The reaction solution was basified with an aqueous potassium carbonate solution, then extracted with chloroform, and the extract was dried over anhydrous magnesium sulfate. The solvent was distilled off, and the residue was purified with a basic silica gel column to give the title compound (0.13 g) as a white powder.

後処理

  1. additionthe mixture was mixed at room temperature for 16 hours
  2. extractionextracted with chloroform
  3. dry with materialthe extract was dried over anhydrous magnesium sulfate
  4. distillationThe solvent was distilled off
  5. customthe residue was purified with a basic silica gel column

出典と根拠

ORDレコード
ord-c46f2e1a308a4935b48dc3efa5d19905
出典データセット
uspto-grants-2009_05
特許番号
US07534887B2

関連ノート

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