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Diisopropylethylamine → 7-(3-Methanesulphonylpyridin-2-yl)-N-(5-(trifluoromethyl)pyridin-2-yl)-5,6,7,8-tetrahydropyrido[3,4-d]pyrimidin-4-amine

HRID 971221
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인쇄 미리보기

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HRID 971221 반응식
[F:1][C:2]([F:21])([F:20])[C:3]1[CH:4]=[CH:5][C:6]([NH:9][C:10]2[C:11]3[CH2:19][CH2:18][NH:17][CH2:16][C:12]=3[N:13]=[CH:14][N:15]=2)=[N:7][CH:8]=1.Cl[C:23]1[C:28]([S:29]([CH3:32])(=[O:31])=[O:30])=[CH:27][CH:26]=[CH:25][N:24]=1.C(N(CC)C(C)C)(C)C>C(#N)C>[CH3:32][S:29]([C:28]1[C:23]([N:17]2[CH2:18][CH2:19][C:11]3[C:10]([NH:9][C:6]4[CH:5]=[CH:4][C:3]([C:2]([F:20])([F:1])[F:21])=[CH:8][N:7]=4)=[N:15][CH:14]=[N:13][C:12]=3[CH2:16]2)=[N:24][CH:25]=[CH:26][CH:27]=1)(=[O:31])=[O:30]
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참가 물질

5

반응물 3

HCID 81531DiisopropylethylamineHCID 125137462-Chloro-3-(methanesulfonyl)pyridineHCID 69424206N-(5-(Trifluoromethyl)pyridine-2-yl)-5,6,7,8-tetrahydropyrido[3,4-d]pyrimidin-4-amine

생성물 1

HCID 694250497-(3-Methanesulphonylpyridin-2-yl)-N-(5-(trifluoromethyl)pyridin-2-yl)-5,6,7,8-tetrahydropyrido[3,4-d]pyrimidin-4-amine수율 43.1%

시약·촉매·용매 1

HCID 6342
Acetonitrile
용매

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온도
150 °C

실험 절차

N-(5-(Trifluoromethyl)pyridine-2-yl)-5,6,7,8-tetrahydropyrido[3,4-d]pyrimidin-4-amine (100 mg, 0.34 mmol) was dissolved in a mixture of acetonitrile (2 mL). To the mixture was added 2-chloro-3-methanesulphonylpyridine (122 mg, 0.68 mmol) and N,N-diisopropylethylamine (0.23 mL, 0.68 mmol). The mixture was heated in a sealed tube at 150° C. in microwave (Model, Personal Chemistry) for 16 h. The solvents were removed under vacuum and the residue was dissolved in ethyl acetate and washed with sat. NaHCO3 and brine. The organic layer was dried over Na2SO4, filtered and evaporated to give a brown residue. The residue was purified by flash chromatography over silica gel using a gradient of ethyl acetate:hexane (0-100%) to give the desired compound as an off-white powder (66 mg).

후처리

  1. customThe solvents were removed under vacuum
  2. dissolutionthe residue was dissolved in ethyl acetate
  3. washwashed with sat. NaHCO3 and brine
  4. dry with materialThe organic layer was dried over Na2SO4
  5. filtrationfiltered
  6. customevaporated
  7. customto give a brown residue
  8. customThe residue was purified by flash chromatography over silica gel using a gradient of ethyl acetate

출처 및 근거

ORD 기록
ord-3d190dcfdce146a79af2b02db42e6e9b
출처 데이터셋
uspto-grants-2007_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07312330B2

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