Ethyl Acetate → HCID 22101898、化合物

HRID 1458301ノート

反応式

HRID 1458301 の反応式
[CH2:1]([N:3]1[CH2:7][CH:6]([NH:8][C:9](=O)[C:10]2[CH:15]=[CH:14][C:13]([O:16][CH2:17]/[CH:18]=[C:19](/[CH2:21][CH2:22][CH:23]=[C:24]([CH3:26])[CH3:25])\[CH3:20])=[CH:12][CH:11]=2)[CH2:5][N:4]1[CH2:28][CH3:29])[CH3:2].COC1C=CC(P2(SP(C3C=CC(OC)=CC=3)(=S)S2)=[S:39])=CC=1.C(OCC)(=O)C>C1(C)C=CC=CC=1>[CH2:1]([N:3]1[CH2:7][CH:6]([NH:8][C:9](=[S:39])[C:10]2[CH:15]=[CH:14][C:13]([O:16][CH2:17]/[CH:18]=[C:19](/[CH2:21][CH2:22][CH:23]=[C:24]([CH3:26])[CH3:25])\[CH3:20])=[CH:12][CH:11]=2)[CH2:5][N:4]1[CH2:28][CH3:29])[CH3:2]

参加物

5

反応物 3

HCID 8857Ethyl AcetateHCID 87949Lawesson's reagentHCID 9908920HCID 9908920、化合物

生成物 1

HCID 22101898HCID 22101898、化合物収率 139.6%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

To a solution of N-(1,2-diethyl-4-pyrazolidinyl)-4-geranyloxybenzamide (1.50 g) in toluene (50 ml) was added Lawesson's reagent (0.76 g). After the reaction solution was refluxed with heating for 30 minutes, ethyl acetate was added thereto. Then, the reaction solution was washed with aqueous sodium bicarbonate solution and then with brine. Its organic layer was concentrated under a vacuum and thus obtained residue was pulled by silica gel column chromatography (chloroform:methanol=30:1), thereby yielding 1.09 g (70%) of the aimed compound.

後処理

  1. temperatureAfter the reaction solution was refluxed
  2. temperaturewith heating for 30 minutes
  3. washThen, the reaction solution was washed with aqueous sodium bicarbonate solution
  4. concentrationIts organic layer was concentrated under a vacuum and thus obtained residue

出典と根拠

ORDレコード
ord-6cc1e6f157c44da3a5f6ba11aa749b8c
出典データセット
uspto-grants-1998_12
特許番号
US05849930

反応ノート

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