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

HRID 1048750노트

반응식

HRID 1048750 반응식
[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

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 23668193Sodium Nitrite2회HCID 866805543-Amino-6-iodopyrazine-2-carbonitrile

생성물 1

HCID 866805553-Chloro-6-iodopyrazine-2-carbonitrile수율 44%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
-50 °C

실험 절차

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.

후처리

  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.

출처 및 근거

ORD 기록
ord-02da375b18d64c65910e47b922e5f331
출처 데이터셋
uspto-grants-2016_07
특허 번호
US09381195B2

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