Ethyl Acetate → HCID 22101898, 화합물

HRID 1458301노트

반응식

HRID 1458301 반응식
[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]

참가 물질

5

반응물 3

HCID 8857Ethyl AcetateHCID 87949Lawesson's reagentHCID 9908920HCID 9908920, 화합물

생성물 1

HCID 22101898HCID 22101898, 화합물수율 139.6%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-6cc1e6f157c44da3a5f6ba11aa749b8c
출처 데이터셋
uspto-grants-1998_12
특허 번호
US05849930

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