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Dimethylformamide → 2-Chloro-4-[4-(2,2,4,6,7-pentamethyl-2,3-dihydro-1-benzofuran-5-yl)piperazin-1-yl]pyrimidine

HRID 2063894
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HRID 2063894 반응식
CN(C=O)C.[CH3:6][C:7]1([CH3:25])[CH2:11][C:10]2[C:12]([CH3:24])=[C:13]([N:18]3[CH2:23][CH2:22][NH:21][CH2:20][CH2:19]3)[C:14]([CH3:17])=[C:15]([CH3:16])[C:9]=2[O:8]1.[Cl:26][C:27]1[N:32]=[C:31]([Cl:33])[CH:30]=[CH:29][N:28]=1.C(N(CC)CC)C>O>[Cl:26][C:27]1[N:32]=[C:31]([N:21]2[CH2:20][CH2:19][N:18]([C:13]3[C:14]([CH3:17])=[C:15]([CH3:16])[C:9]4[O:8][C:7]([CH3:25])([CH3:6])[CH2:11][C:10]=4[C:12]=3[CH3:24])[CH2:23][CH2:22]2)[CH:30]=[CH:29][N:28]=1.[Cl:33][C:31]1[CH:30]=[CH:29][N:28]=[C:27]([N:21]2[CH2:20][CH2:19][N:18]([C:13]3[C:14]([CH3:17])=[C:15]([CH3:16])[C:9]4[O:8][C:7]([CH3:25])([CH3:6])[CH2:11][C:10]=4[C:12]=3[CH3:24])[CH2:23][CH2:22]2)[N:32]=1
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참가 물질

7

반응물 4

HCID 6228DimethylformamideHCID 8471TriethylamineHCID 775312,4-DichloropyrimidineHCID 667597311-(2,2,4,6,7-Pentamethyl-2,3-dihydro-1-benzofuran-5-yl)piperazine

생성물 2

HCID 594850032-Chloro-4-[4-(2,2,4,6,7-pentamethyl-2,3-dihydro-1-benzofuran-5-yl)piperazin-1-yl]pyrimidine수율 62%
HCID 59485115
4-Chloro-2-[4-(2,2,4,6,7-pentamethyl-2,3-dihydro-1-benzofuran-5-yl)piperazin-1-yl]pyrimidine
수율 4%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To the DMF (10 mL) solution of 1-(2,2,4,6,7-pentamethyl-2,3-dihydro-1-benzofuran-5-yl)piperazine (1.92 g, 7.00 mmol) synthesized in Reference example 61, 2,4-dichloropyrimidine (1.04 g, 7.00 mmol) and triethylamine (1.07 mL, 7.70 mmol) were added and the mixture was stirred at room temperature for 1 hour. To the mixture solution, water was added. The extraction was carried out by using ethyl acetate, and the extract was dried over anhydrous magnesium sulfate. Then, the solvent was removed by distillation under reduced pressure. The resulting residue was purified by silica gel column chromatography (hexane-ethyl acetate 95:5-85:15) to obtain 2-chloro-4-[4-(2,2,4,6,7-pentamethyl-2,3-dihydro-1-benzofuran-5-yl)piperazin-1-yl]pyrimidine 1.68 g (ethyl acetate/hexane=4:1, Rf=0.1, yield 62%) and 4-chloro-2-[4-(2,2,4,6,7-pentamethyl-2,3-dihydro-1-benzofuran-5-yl)piperazin-1-yl]pyrimidine 100 mg (ethyl acetate/hexane=4:1, Rf=0.5, yield 4%).

후처리

  1. additionwere added
  2. extractionThe extraction
  3. dry with materialthe extract was dried over anhydrous magnesium sulfate
  4. customThen, the solvent was removed by distillation under reduced pressure
  5. customThe resulting residue was purified by silica gel column chromatography (hexane-ethyl acetate 95:5-85:15)

출처 및 근거

ORD 기록
ord-7c42e55cf1d14039ae90725260a79b90
출처 데이터셋
uspto-grants-2012_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08288390B2

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