Hydrochloric Acid → 3-Chloro-6-iodopyrazine-2-carbonitrile

HRID 1487357ノート

反応式

HRID 1487357 の反応式
[ClH:1].N[C:3]1[C:4]([C:10]#[N:11])=[N:5][C:6]([I:9])=[CH:7][N:8]=1.N([O-])=O.[Na+]>O>[Cl:1][C:3]1[C:4]([C:10]#[N:11])=[N:5][C:6]([I:9])=[CH:7][N:8]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 23668193Sodium Nitrite2 回HCID 866805543-Amino-6-iodopyrazine-2-carbonitrile

生成物 1

HCID 866805553-Chloro-6-iodopyrazine-2-carbonitrile収率 44%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
-50 °C

実験手順

64.3 ml of hydrochloric acid is added at −5° C. to 7.7 g (31.3 mmol) of 3-amino-6-iodopyrazine-2-carbonitrile. At this temperature, a sodium nitrite solution (4.32 g, 62.6 mmol) dissolved in 9 ml of water is added to the reaction mixture and is stirred for 4 hours at −50° C. and then at room temperature overnight. Another equivalent of sodium nitrite is added to the reaction mixture and the precipitate formed is filtered, rinsed with water and dried at 50° C. to yield 3.65 g (44%) of 3-chloro-6-iodopyrazine-2-carbonitrile in the form of a beige solid.

後処理

  1. additionis added to the reaction mixture
  2. customat room temperature
  3. customovernight
  4. customthe precipitate formed
  5. filtrationis filtered
  6. washrinsed with water
  7. customdried at 50° C.

出典と根拠

ORDレコード
ord-f93cbc89c4664bffb5fa957a5b8f1248
出典データセット
uspto-grants-2016_08
特許番号
US09428510B2

反応ノート

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