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Pyrrolidine → (E)-2-[2-(3-Chloro-phenyl)-vinyl]-4-methyl-6-pyrrolidin-1-yl-pyrimidine

HRID 431237
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인쇄 미리보기

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HRID 431237 반응식
[CH3:1][C:2]1[N:7]=[C:6](/[CH:8]=[CH:9]/[C:10]2[CH:15]=[CH:14][CH:13]=[C:12](C(F)(F)F)[CH:11]=2)[N:5]=[C:4]([N:20]2[CH2:29][CH2:28][C:27]3[C:22](=CC=CC=3)C2)[CH:3]=1.[Cl:30]C1C=C(C)N=C(C=CC2C=CC=C(Cl)C=2)N=1.N1CCCC1>C(Cl)Cl.CCOC(C)=O>[Cl:30][C:12]1[CH:11]=[C:10](/[CH:9]=[CH:8]/[C:6]2[N:7]=[C:2]([CH3:1])[CH:3]=[C:4]([N:20]3[CH2:29][CH2:28][CH2:27][CH2:22]3)[N:5]=2)[CH:15]=[CH:14][CH:13]=1
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참가 물질

5

반응물 3

HCID 31268PyrrolidineHCID 18763632(E)-2-{6-methyl-2-[2-(3-trifluoromethyl-phenyl)-vinyl]-pyrimidin-4-yl}-1,2,3,4-tetrahydro-isoquinolineHCID 734621854-Chloro-2-[2-(3-chloro-phenyl)-vinyl]-6-methyl-pyrimidine

생성물 1

HCID 9835946(E)-2-[2-(3-Chloro-phenyl)-vinyl]-4-methyl-6-pyrrolidin-1-yl-pyrimidine수율 80%

시약·촉매·용매 1

HCID 21226138
Dichloromethane ethylacetate
용매

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온도
60 °C

실험 절차

A mixture of 66 mg (0.25 mmol) of (E) 4-chloro-2-[2-(3-chloro-phenyl)-vinyl]-6-methyl-pyrimidine and 0.89 g (12.5 mmol) pyrrolidine was heated at 60° C. for 1.5 h after which time the reaction was completed according to TLC analysis (CH2Cl2/EtOAc: 4/1). The excess pyrrolidine was removed in vacuo and the residue was purified on a silica gel chromatography column (eluted with CH2Cl2/EtOAc: 4/1). The purified fractions were combined, evacuated in vacuo, the solid residue was triturated with ether and filtered off by suction to give (E)-2-[2-(3-Chloro-phenyl)-vinyl]-4-methyl-6-pyrrolidin-1-yl-pyrimidine (61 mg, 80%) as an off-white crystalline solid. ISP mass spectrum, m/e: 300.3 (M+1 calculated for C17H18ClN3: 300).

후처리

  1. customThe excess pyrrolidine was removed in vacuo
  2. customthe residue was purified on a silica gel chromatography column (eluted with CH2Cl2/EtOAc: 4/1)
  3. customevacuated in vacuo
  4. customthe solid residue was triturated with ether
  5. filtrationfiltered off by suction

출처 및 근거

ORD 기록
ord-af9e1104b7c1445bb08a23a6a174d4bc
출처 데이터셋
uspto-grants-2003_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06657060B2

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