Hydrazine hydrate (1:1) → 3-Amino-6-bromopyrazine-2-carbohydrazide

HRID 78726

반응식

HRID 78726 반응식
[NH2:1][C:2]1[C:3]([C:9]([O:11]C)=O)=[N:4][C:5]([Br:8])=[CH:6][N:7]=1.O.[NH2:14][NH2:15]>O1CCOCC1>[NH2:1][C:2]1[C:3]([C:9]([NH:14][NH2:15])=[O:11])=[N:4][C:5]([Br:8])=[CH:6][N:7]=1

참가 물질

4

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 227251Methyl 3-Amino-6-bromopyrazine-2-carboxylate

생성물 1

HCID 580702563-Amino-6-bromopyrazine-2-carbohydrazide

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

반응 조건

온도
60 °C

실험 절차

Methyl 3-amino-6-bromopyrazine-2-carboxylate (15 g, 64.6 mmol) was suspended in 150 mL of dioxane at room temperature. Hydrazine hydrate (6.5 g, 130 mmol) was added and the reaction mixture was stirred at 60° C. for 2 hours. Initially the mixture became clear, but after a while a precipitate formed. The mixture was cooled to ambient temperature and crude product filtered off. The solid was washed with TBME and subsequently stirred in water. The material was filtered and washed with acetone to afford 3-Amino-6-bromopyrazine-2-carbohydrazide 4 as slightly yellow solid. The material was dried in vacuo. (10.5 g, 70%).

후처리

  1. customafter a while a precipitate formed
  2. temperatureThe mixture was cooled to ambient temperature
  3. filtrationcrude product filtered off
  4. washThe solid was washed with TBME
  5. stirringsubsequently stirred in water
  6. filtrationThe material was filtered
  7. washwashed with acetone

출처 및 근거

ORD 기록
ord-be4ae37bcf25498c950d1b45beb2a192
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08841449B2

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