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Ammonia → 6-Chloro-5-methylpyridazin-3-amine

HRID 2279071
ノート
印刷プレビュー

反応式

HRID 2279071 の反応式
[NH3:1].[Cl:2][C:3]1[N:4]=[N:5][C:6](Cl)=[CH:7][C:8]=1[CH3:9]>C(O)C>[Cl:2][C:3]1[N:4]=[N:5][C:6]([NH2:1])=[CH:7][C:8]=1[CH3:9]
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

4

反応物 2

HCID 222AmmoniaHCID 879233,6-Dichloro-4-methylpyridazine

生成物 1

HCID 123536636-Chloro-5-methylpyridazin-3-amine収率 57%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
100 °C

実験手順

Ammonia (32% solution in water, 54 mL) was added to a solution of 3,6-dichloro-4-methylpyridazine (5.0 g, 30.67 mmol) in ethanol (25 mL) in a sealed tube. The resulting mixture was stirred at 100° C. for 70 hours, cooled down and the solvent was removed under reduced pressure. The residue was purified by flash chromatography (3:2 hexanes/ethyl acetate to 100% ethyl acetate) to yield the title compound (3.8 g, 57%) as a mixture of two isomers which was used in the next step without further purification.

後処理

  1. temperaturecooled down
  2. customthe solvent was removed under reduced pressure
  3. customThe residue was purified by flash chromatography (3:2 hexanes/ethyl acetate to 100% ethyl acetate)

出典と根拠

ORDレコード
ord-ec512ba95bcd4741a25a5a1a0c7f6954
出典データセット
uspto-grants-2015_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09133200B2

反応ノート

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