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Dimethyl acetylsuccinate → HCID 178499487, 화합물

HRID 472827
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HRID 472827 반응식
[Br:1][C:2]1[CH:6]=[C:5]([NH2:7])[NH:4][N:3]=1.[C:8]([CH:11]([CH2:16][C:17]([O:19][CH3:20])=[O:18])[C:12](OC)=[O:13])(=O)[CH3:9].O.C1(C)C=CC(S(O)(=O)=O)=CC=1>C1(C)C(C)=CC=CC=1>[Br:1][C:2]1[CH:6]=[C:5]2[N:7]=[C:8]([CH3:9])[C:11]([CH2:16][C:17]([O:19][CH3:20])=[O:18])=[C:12]([OH:13])[N:4]2[N:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 112039Dimethyl acetylsuccinateHCID 521998p-Toluenesulfonic acid monohydrateHCID 178507227HCID 178507227, 화합물

생성물 1

HCID 178499487HCID 178499487, 화합물수율 54.2%

시약·촉매·용매 1

HCID 7237O-Xylene용매

실험 절차

To a solution of 3-bromo-1H-pyrazol-5-amine (0.2 g, 1.235 mmol) and dimethyl 2-acetylsuccinate (0.697 g, 3.70 mmol) in xylene (10 mL) was added p-toluenesulfonic acid monohydrate (2 mg, 10.51 mmol). The reaction mixture was heated at reflux under a Dean-Stark trap for 8 h. The solid was filtered and washed with hexanes to afford the title compound (0.201 g, 54.2%). 1H NMR (400 MHz, MeOD) δ ppm 2.37 (3H, s), 3.65 (2H, s), 3.71 (3H, s), 6.20 (1H, s).

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후처리

  1. temperatureThe reaction mixture was heated
  2. temperatureat reflux under a Dean-Stark trap for 8 h
  3. filtrationThe solid was filtered
  4. washwashed with hexanes

출처 및 근거

ORD 기록
ord-39c0c42f58844b328b9160f0e8ea4d33
출처 데이터셋
uspto-grants-2014_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08633200B2

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