2(1H)-Quinoxalinone, 3,4-dihydro- → 4-Nitroso-3,4-dihydroquinoxalin-2(1H)-one

HRID 717765

反応式

HRID 717765 の反応式
[NH:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[NH:4][CH2:3][C:2]1=[O:11].[N:12]([O-])=[O:13].[Na+]>Cl.O>[N:12]([N:4]1[C:5]2[C:10](=[CH:9][CH:8]=[CH:7][CH:6]=2)[NH:1][C:2](=[O:11])[CH2:3]1)=[O:13]

参加物

5

反応物 2

HCID 1859492(1H)-Quinoxalinone, 3,4-dihydro-HCID 23668193Sodium Nitrite

生成物 1

HCID 131503004-Nitroso-3,4-dihydroquinoxalin-2(1H)-one収率 66.8%

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid溶媒HCID 962Water溶媒2 回

反応条件

温度
0 °C

実験手順

3,4-Dihydro-1H-quinoxalin-2-one (500 mg, 3.378 mmol) was dissolved in 3N HCl (10 mL) and stirred for 5 min. at 0° C. A solution of sodium nitrite (256 mg, 3.716 mmol) in water (2 mL) was added at 0° C., and the reaction mixture was stirred for 2 h at RT. After completion of reaction, water was added and the mixture extracted twice with DCM (100 mL). The combined organic layers were washed with water, dried over sodium sulfate and concentrated under reduced pressure to obtain 400 mg of 3,4-dihydro-4-nitrosoquinoxalin-2(1H)-one.

後処理

  1. stirringthe reaction mixture was stirred for 2 h at RT
  2. additionwas added
  3. extractionthe mixture extracted twice with DCM (100 mL)
  4. washThe combined organic layers were washed with water
  5. dry with materialdried over sodium sulfate
  6. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-24f5d11fe391424b8550b68b20cabb37
出典データセット
uspto-grants-2015_11
特許番号
US09193728B2

関連ノート

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