Hydrazine hydrate (1:1) → Pyrazine-2-Carboxylic Acid Hydrazide

HRID 30341

반응식

HRID 30341 반응식
C[O:2][C:3]([C:5]1[CH:10]=[N:9][CH:8]=[CH:7][N:6]=1)=O.O.[NH2:12][NH2:13]>CCO>[N:6]1[CH:7]=[CH:8][N:9]=[CH:10][C:5]=1[C:3]([NH:12][NH2:13])=[O:2]

참가 물질

4

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 72662Methyl pyrazinoate

생성물 1

HCID 258796Pyrazine-2-Carboxylic Acid Hydrazide수율 100.5%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a stirred solution of pyrazine-2-carboxylic acid methyl ester (11.1 g, 80 mmol) in 140 mL of EtOH was added hydrazine hydrate (15.6 mL, 320 mmol). The resultant solution was heated to reflux for 2 h. The solvent was removed under reduced pressure and dried under high vacuum to yield the title amide (11.1 g, 100%) as a white solid. The product was used in subsequent steps without purification. 1H NMR (d6-DMSO δ 10.1, br s, 1H; δ 9.12, d, 1H; δ 8.83, d, 1H; δ 8.70, dd, 1H; δ 4.64, br s, 2H), LC/MS (APCI, ES, M+H=139).

후처리

  1. temperatureto reflux for 2 h
  2. customThe solvent was removed under reduced pressure
  3. customdried under high vacuum

출처 및 근거

ORD 기록
ord-35609971f8c649e199cbfff87dfa3bc1
출처 데이터셋
uspto-grants-2008_09
특허 번호
US07423061B2

연결된 노트

불러오는 중…