Phosphorus oxychloride → 2-Chloro-3-(2-thienyl)quinoxaline

HRID 553452

反応式

HRID 553452 の反応式
[S:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[C:6]1[C:7](=O)[NH:8][C:9]2[C:14]([N:15]=1)=[CH:13][CH:12]=[CH:11][CH:10]=2.O=P(Cl)(Cl)[Cl:19]>>[Cl:19][C:7]1[C:6]([C:2]2[S:1][CH:5]=[CH:4][CH:3]=2)=[N:15][C:14]2[C:9](=[CH:10][CH:11]=[CH:12][CH:13]=2)[N:8]=1

参加物

3

反応物 2

HCID 24813Phosphorus oxychlorideHCID 7236983-(2-Thienyl)-1,2-dihydroquinoxalin-2-one

生成物 1

HCID 28016552-Chloro-3-(2-thienyl)quinoxaline収率 74%

反応条件

温度
120 °C

実験手順

A mixture of 3-(2-thienyl)quinoxalin-2(1 H)-one (500 mg, 2.19 mmol.) and POCl3 (6 mL) was heated to reflux at 120° C. After the material was consumed, the reaction mixture was taken up with water and ice. The solid was collected and dried in vacuo to give 2-chloro-3-(2-thienyl)quinoxaline (400 mg, 74%). 1 H NMR (400 MHz, CDCl3) δ 8.22 (d, J=4.8 Hz, 1 H), 8.00 (d, J=10.4 Hz, 1 H), 7.91 (d, J=10.4 Hz, 1 H), 7.72˜7.61 (m, 2 H), 7.52 (d, J=6.8 Hz, 1 H), 7.13 (t, J=6.0 Hz, 1 H).

後処理

  1. temperaturewas heated
  2. customAfter the material was consumed
  3. customThe solid was collected
  4. customdried in vacuo

出典と根拠

ORDレコード
ord-0d832703f8194eceb3554f988077721c
出典データセット
uspto-grants-2011_11
特許番号
US08048862B2

関連ノート

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