9-(6-Chloro-2-(4-nitrophenyl)pyrimidin-4-yl)-3,7-dioxa-9-azabicyclo[3.3.1]nonane → HCID 66750356、化合物

HRID 75454ノート

反応式

HRID 75454 の反応式
Cl[C:2]1[N:7]=[C:6]([C:8]2[CH:13]=[CH:12][C:11]([N+:14]([O-:16])=[O:15])=[CH:10][CH:9]=2)[N:5]=[C:4]([N:17]2[CH:22]3[CH2:23][O:24][CH2:25][CH:18]2[CH2:19][O:20][CH2:21]3)[CH:3]=1>C(N)(C)C>[CH:22]12[N:17]([C:4]3[N:5]=[C:6]([C:8]4[CH:13]=[CH:12][C:11]([N+:14]([O-:16])=[O:15])=[CH:10][CH:9]=4)[N:7]=[C:2]([NH:14][CH:11]([CH3:12])[CH3:10])[CH:3]=3)[CH:18]([CH2:25][O:24][CH2:23]1)[CH2:19][O:20][CH2:21]2

参加物

3

反応物 1

HCID 866659039-(6-Chloro-2-(4-nitrophenyl)pyrimidin-4-yl)-3,7-dioxa-9-azabicyclo[3.3.1]nonane

生成物 1

HCID 66750356HCID 66750356、化合物収率 198.6%

試薬・触媒・溶媒 1

HCID 6363Isopropylamine溶媒

反応条件

温度
145 °C

実験手順

In a 2-5 mL microwave vial was placed 9-(6-chloro-2-(4-nitrophenyl)pyrimidin-4-yl)-3,7-dioxa-9-azabicyclo[3.3.1]nonane (130 mg, 0.358 mmol) in isopropylamine (5 mL) to give a yellow suspension. The reaction was heated under microwave irradiation at 145° C. for 60 min. The mixture was concentrated. The residue was dissolved in dichloromethane and washed with saturated NaHCO3. The organic phase was dried (MgSO4), filtered and concentrated to give 137 mg (99%) of a yellow foam. HRMS: 386.1824 [M+H]+. For [M+H]+ mass error=0.1 mDa or 0.21 ppm.

後処理

  1. customto give a yellow suspension
  2. concentrationThe mixture was concentrated
  3. dissolutionThe residue was dissolved in dichloromethane
  4. washwashed with saturated NaHCO3
  5. dry with materialThe organic phase was dried (MgSO4)
  6. filtrationfiltered
  7. concentrationconcentrated

出典と根拠

ORDレコード
ord-3fca1d644e9a48ad966b12bef025fdb2
出典データセット
uspto-grants-2014_09
特許番号
US08835429B2

反応ノート

読み込み中…