Diisopropylethylamine → HCID 178516733, 화합물

HRID 454337노트

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HRID 454337 반응식
Br[C:2]1[N:3]=[C:4]2[N:11]([CH:12]3[CH2:17][CH2:16][O:15][CH2:14][CH2:13]3)[CH2:10][C:9](=[O:18])[NH:8][C:5]2=[N:6][CH:7]=1.Br[C:20]1[C:21]([NH:27][C:28](=O)CI)=[N:22][CH:23]=[C:24](Br)[N:25]=1.[CH:32](N(C(C)C)CC)(C)[CH3:33].O1CCC([NH2:47])CC1>C(#N)C>[NH:47]1[CH:28]=[N:27][C:21]([C:20]2[N:25]=[CH:24][C:23]([C:2]3[N:3]=[C:4]4[N:11]([CH:12]5[CH2:17][CH2:16][O:15][CH2:14][CH2:13]5)[CH2:10][C:9](=[O:18])[NH:8][C:5]4=[N:6][CH:7]=3)=[CH:33][CH:32]=2)=[N:22]1

참가 물질

6

반응물 4

HCID 81531DiisopropylethylamineHCID 4192234-AminotetrahydropyranHCID 58298325N-(3,5-dibromopyrazin-2-yl)-2-iodoacetamideHCID 866446486-Bromo-4-(tetrahydro-2H-pyran-4-yl)-3,4-dihydropyrazino[2,3-b]pyrazin-2(1H)-one

생성물 1

HCID 178516733HCID 178516733, 화합물수율 40%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

6-Bromo-4-(tetrahydro-2H-pyran-4-yl)-3,4-dihydropyrazino[2,3-b]pyrazin-2(1H)-one. To a solution of N-(3,5-dibromopyrazin-2-yl)-2-iodoacetamide (See Example 5.B) (6.6 g, 15.8 mmol) and diisopropylethylamine (4.0 g, 31.6 mmol) in acetonitrile (50 mL) was added tetrahydro-2H-pyran-4-amine (6.4 g, 63.2 mmol) and the mixture was stirred at ambient temperature for 16 h. The solvent was removed under reduced pressure and the residue which was purified by chromatography on silica gel (5-20% ethyl acetate in petroleum ether) to give the title compound (1.98 g, 40% yield). MS (ESI) m/z 313.1 [M+1]+.

후처리

  1. customThe solvent was removed under reduced pressure
  2. customthe residue which was purified by chromatography on silica gel (5-20% ethyl acetate in petroleum ether)

출처 및 근거

ORD 기록
ord-c24c9e23b8c04cfa9b32d6a5242c8782
출처 데이터셋
uspto-grants-2013_07
특허 번호
US08492381B2

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