Ammonium Chloride → 1013117-35-5

HRID 2405758ノート

反応式

HRID 2405758 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][C:11]=1[N+:12]([O-])=O)[N:8]=[CH:7][NH:6][C:5]2=[O:15].[NH4+].[Cl-]>CO.O.[Fe]>[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][C:11]=1[NH2:12])[N:8]=[CH:7][NH:6][C:5]2=[O:15]

参加物

6

反応物 2

HCID 25517Ammonium ChlorideHCID 135767899HCID 135767899、化合物

生成物 1

HCID 1360138721013117-35-5収率 100.7%

試薬・触媒・溶媒 3

HCID 23925Iron触媒HCID 887Methanol溶媒HCID 962Water溶媒

反応条件

温度
65 °C

実験手順

To a suspension of 6-chloro-7-nitroquinazoline-4-one (7.5 g, 33 mmol) in MeOH (250 mL) was added NH4Cl (17.7 g, 0.33 mol) dissolved in water (75 mL). Iron powder (18.5 g, 330 mmol) was added and the suspension was heated at 65° C. for 2 h. The warm reaction mixture was filtered over diatomaceous earth and washed several times with THF (1 L) and methanol (500 mL). The filtrate was concentrated, washed with water and dried under vacuum at 50° C. to afford the title compound (6.5 g, 90%) as a brown solid. ESI-MS m/z 196 [C8H6ClN3O+H]+.

後処理

  1. customThe warm reaction mixture
  2. filtrationwas filtered over diatomaceous earth
  3. washwashed several times with THF (1 L) and methanol (500 mL)
  4. concentrationThe filtrate was concentrated
  5. washwashed with water
  6. customdried under vacuum at 50° C.

出典と根拠

ORDレコード
ord-a111bca80fd34374af0fd0545523b698
出典データセット
uspto-grants-2014_08
特許番号
US08809326B2

反応ノート

読み込み中…