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Diisopropylethylamine → 4-[(1,3-Dithiolan-2-yl)-methyl]amino-5,6-diphenyl furo[2,3-d]pyrimidine

HRID 502657
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HRID 502657 반응식
Br[C:2]1[C:3]2[C:10]([C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=3)=[C:9]([C:17]3[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=3)[O:8][C:4]=2[N:5]=[CH:6][N:7]=1.[S:23]1[CH2:27][CH2:26][S:25][CH:24]1NC.C[CH2:31][N:32](C(C)C)C(C)C>C(O)CCC>[S:25]1[CH2:26][CH2:27][S:23][CH:24]1[CH2:31][NH:32][C:2]1[C:3]2[C:10]([C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=3)=[C:9]([C:17]3[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=3)[O:8][C:4]=2[N:5]=[CH:6][N:7]=1
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참가 물질

5

반응물 3

HCID 81531DiisopropylethylamineHCID 586033114-Bromo-5,6-diphenyl-furo[2,3-d]pyrimidineHCID 866032271,3-Dithiolan-2-yl-methylamine

생성물 1

HCID 860887714-[(1,3-Dithiolan-2-yl)-methyl]amino-5,6-diphenyl furo[2,3-d]pyrimidine수율 34.7%

시약·촉매·용매 1

HCID 2631-Butanol용매

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온도
120 °C

실험 절차

A mixture of 69 (150 mg, 0.86 mmol), 1,3-dithiolan-2-yl-methylamine (240 μL, 1.78 mmol), and DIEA 0.31 mL (1.78 mmol) in 1-butanol (1 mL) was heated to 120° C. for 2 h. After cooling, the reaction mixture was concentrated, and the residue was purified by silica gel column chromatography, affording 110 (121 mg). LCMS and 1HNMR are identical with the product obtained from method 1.

후처리

  1. temperatureAfter cooling
  2. concentrationthe reaction mixture was concentrated
  3. customthe residue was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-dcf7bbea9429499eb6e26c15bf6ea122
출처 데이터셋
uspto-grants-2010_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07776867B2

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