Hydrochloric Acid → (S)-1-acetyl-2-methyl-4-nitrosopiperazine

HRID 1596209ノート

反応式

HRID 1596209 の反応式
[C:1]([N:4]1[CH2:9][CH2:8][NH:7][CH2:6][C@@H:5]1[CH3:10])(=[O:3])[CH3:2].Cl.[N:12]([O-])=[O:13].[Na+].[OH-].[Na+]>O>[C:1]([N:4]1[CH2:9][CH2:8][N:7]([N:12]=[O:13])[CH2:6][C@@H:5]1[CH3:10])(=[O:3])[CH3:2]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 23668193Sodium NitriteHCID 54446440(2S)-N-acetyl-2-methylpiperazine

生成物 1

HCID 45085766(S)-1-acetyl-2-methyl-4-nitrosopiperazine収率 68.6%

試薬・触媒・溶媒 1

HCID 962Water溶媒3 回

反応条件

温度
0 °C

実験手順

To a slurry of (S)-1-acetyl-2-methylpiperazine (424 mg) in water (2.5 ml) was added concentrated hydrochloric acid (0.9 ml) dropwise below 25° C. A solution of sodium nitrite (227 mg) in water (2 ml) was added dropwise at 0° C. The mixture was stirred at 0° C. for 2 hours. A solution of sodium hydroxide (409 mg) in water (6 ml) was added dropwise at 0° C. The mixture was extracted with chloroform, washed with water, dried and evaporated to give (S)-1-acetyl-2-methyl-4-nitrosopiperazine (350 mg). This product was used for next step without purification.

後処理

  1. extractionThe mixture was extracted with chloroform
  2. washwashed with water
  3. customdried
  4. customevaporated

出典と根拠

ORDレコード
ord-2db1d6d7dcb8418f837c126d3bcfd1db
出典データセット
uspto-grants-2001_09
特許番号
US06291464B1

反応ノート

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