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3-Isocyanatopyridine → US9296747, Example 3

HRID 930502
ノート
印刷プレビュー

反応式

HRID 930502 の反応式
[C:1]1([NH:7][C:8]2[N:9]=[CH:10][C:11]3[CH2:17][NH:16][CH2:15][CH2:14][C:12]=3[N:13]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[N:18]([C:21]1[CH:22]=[N:23][CH:24]=[CH:25][CH:26]=1)=[C:19]=[O:20]>C(Cl)Cl>[NH:7]([C:8]1[N:9]=[CH:10][C:11]2[CH2:17][N:16]([C:19]([NH:18][C:21]3[CH:22]=[N:23][CH:24]=[CH:25][CH:26]=3)=[O:20])[CH2:15][CH2:14][C:12]=2[N:13]=1)[C:1]1[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 27604933-IsocyanatopyridineHCID 104609480N-phenyl-5,6,7,8-tetrahydropyrido[4,3-d]pyrimidin-2-amine

生成物 1

HCID 118970906US9296747, Example 3

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

A solution of N-phenyl-5,6,7,8-tetrahydropyrido[4,3-d]pyrimidin-2-amine, Intermediate 6 (75 mg, 0.33 mmol), 3-isocyanatopyridine (41.8 mg, 0.35 mmol) in CH2Cl2 (1.5 mL) was stirred at room temperature for 1 hour. After 1 hour the reaction mixture was diluted with CH2Cl2 and washed with sat. aqueous NaHCO3(aq). The organic phase was collected, dried and concentrated. The residue was dissolved in CH2Cl2 and washed with 3% aqueous LiCl solution and water. The organic phase was collected, dried and concentrated to give the title compound (45.9 mg).

後処理

  1. washwashed with sat. aqueous NaHCO3(aq)
  2. customThe organic phase was collected
  3. customdried
  4. concentrationconcentrated
  5. dissolutionThe residue was dissolved in CH2Cl2
  6. washwashed with 3% aqueous LiCl solution and water
  7. customThe organic phase was collected
  8. customdried
  9. concentrationconcentrated

出典と根拠

ORDレコード
ord-8fb5bbed33ea4f298a56f5d494fdd45f
出典データセット
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09296747B1

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート