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Sodium Hydroxide → 3-Hydrazino-1-methyl-5-methylmercaptopyrazole

HRID 362662
ノート
印刷プレビュー

反応式

HRID 362662 の反応式
[N:1]([O-])=O.[Na+].[NH2:5][C:6]1[CH:10]=[C:9]([S:11][CH3:12])[N:8]([CH3:13])[N:7]=1.O.O.Cl[Sn]Cl.[OH-].[Na+]>O.Cl>[NH:5]([C:6]1[CH:10]=[C:9]([S:11][CH3:12])[N:8]([CH3:13])[N:7]=1)[NH2:1]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 14798Sodium HydroxideHCID 61436Stannous chloride dihydrateHCID 23668193Sodium NitriteHCID 542284381-Methyl-5-(methylthio)-1H-pyrazol-3-amine

生成物 1

HCID 451213143-Hydrazino-1-methyl-5-methylmercaptopyrazole収率 96.5%

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid
溶媒
2 回
HCID 962Water溶媒

反応条件

温度
0 °C

実験手順

1.1 g (15.8 mmol) sodium nitrite in 4 ml water was added dropwise to 1.9 g (13.1 mmol) 3-amino-1-methyl-5-methylmercaptopyrazole in 28 ml concentrated hydrochloric acid at 0° C. and the mixture stirred for 2 hours at 0° C. Then, at -30° C., a solution of 7.4 g (32.8 mmol) SnCl2.2H2O in 5.5 ml concentrated hydrochloric acid was added dropwise and the mixture stirred for 3 hours at this temperature. The reaction mixture was then made basic with 32% caustic soda and extracted with methylene chloride. The organic phase was dried over sodium sulfate and concentrated. 2.0 g of product was obtained which was used without further purification.

後処理

  1. stirringthe mixture stirred for 3 hours at this temperature
  2. extractionextracted with methylene chloride
  3. dry with materialThe organic phase was dried over sodium sulfate
  4. concentrationconcentrated

出典と根拠

ORDレコード
ord-6e4607a14e90497497466146eaf69488
出典データセット
uspto-grants-1999_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05869686

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート