Hydrazine hydrate (1:1) → HCID 178434364, 화합물

HRID 1022223노트

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HRID 1022223 반응식
[Br:1][C:2]1[CH:7]=[C:6]([C:8](=O)[CH3:9])[C:5](F)=[CH:4][N:3]=1.O.[NH2:13][NH2:14]>C(O)CO>[Br:1][C:2]1[CH:7]=[C:6]2[C:8]([CH3:9])=[N:14][NH:13][C:5]2=[CH:4][N:3]=1

참가 물질

4

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 252229461-(2-Bromo-5-fluoropyridin-4-yl)ethan-1-one

생성물 1

HCID 178434364HCID 178434364, 화합물수율 74%

시약·촉매·용매 1

HCID 174Ethylene Glycol용매

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온도
165 °C

실험 절차

To a 250-mL round-bottomed flask equipped with a reflux condenser was added dry ethylene glycol (30 mL) and 325c (4.3 g, 20 mmol). Then hydrazine hydrate (5.0 mL, 4.8 g, 81.6 mmol) was added dropwise via a syringe. The mixture was heated at 165° C. for 3.5 h. The resulting orange-tan mixture was cooled to room temperature and the contents were poured onto a stirring mixture of 100 mL ice/water (1:1), whereupon precipitation occurred. After stirring for 10 min, the off-white precipitate was collected, which was dried in vacuo to afford 325d as an off-white solid (3.1 g, 74%). MS-ESI: [M+H]+ 211.9.

후처리

  1. customTo a 250-mL round-bottomed flask equipped with a reflux condenser
  2. temperatureThe resulting orange-tan mixture was cooled to room temperature
  3. customthe off-white precipitate was collected
  4. customwhich was dried in vacuo

출처 및 근거

ORD 기록
ord-753cc12c16e743138d10b5690f3727d2
출처 데이터셋
uspto-grants-2014_05
특허 번호
US08716274B2

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