Diisopropylethylamine → HCID 178516733、化合物

HRID 1640310ノート

反応式

HRID 1640310 の反応式
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

参加物

6

反応物 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

生成物 1

HCID 178516733HCID 178516733、化合物収率 40%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

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]+.

後処理

  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)

出典と根拠

ORDレコード
ord-d877d01d9dbf442d8f49237878bf720a
出典データセット
uspto-grants-2012_02
特許番号
US08110578B2

反応ノート

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