N-Iodosuccinimide → HCID 178522276、化合物

HRID 2283472ノート

反応式

HRID 2283472 の反応式
[OH:1][C:2]1[C:7]([NH:8][C:9](=[O:18])[O:10][CH2:11][C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)=[CH:6][CH:5]=[CH:4][N:3]=1.C1C(=O)N([I:26])C(=O)C1>C(Cl)Cl>[OH:1][C:2]1[C:7]([NH:8][C:9](=[O:18])[O:10][CH2:11][C:12]2[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=2)=[CH:6][C:5]([I:26])=[CH:4][N:3]=1

参加物

4

反応物 2

HCID 120273N-IodosuccinimideHCID 178522213HCID 178522213、化合物

生成物 1

HCID 178522276HCID 178522276、化合物収率 65.6%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of benzyl (2-hydroxypyridin-3-yl)carbamate (16.1 g, 65.9 mmol) in DCM (500 mL) was added NIS (17.8 g, 79.1 mmol) and the mixture heated at reflux overnight. After cooling, the mixture was filtered to afford benzyl (2-hydroxy-5-iodopyridin-3-yl)carbamate (16 g, 65% yield) as a white solid: 1H NMR (400 MHz, CDCl3) δ 8.27 (s, 1H), 7.72 (s, 1H), 7.29-7.40 (m, 5H), 5.21 (s, 2H); MS (ES) m/z 370 (M+H).

後処理

  1. temperaturethe mixture heated
  2. temperatureat reflux overnight
  3. temperatureAfter cooling
  4. filtrationthe mixture was filtered

出典と根拠

ORDレコード
ord-bc1ecfc34a0b4e7eb537f3f5c8ab71d7
出典データセット
uspto-grants-2015_09
特許番号
US09145393B2

反応ノート

読み込み中…