Hydrazine hydrate (1:1) → HCID 66690636, 화합물

HRID 592296노트

반응식

HRID 592296 반응식
[Cl:1][C:2]1[C:3](Cl)=[N:4][CH:5]=[C:6]([CH:14]=1)[C:7]([O:9][C:10]([CH3:13])([CH3:12])[CH3:11])=[O:8].O.[NH2:17][NH2:18]>C(O)C>[Cl:1][C:2]1[C:3]([NH:17][NH2:18])=[N:4][CH:5]=[C:6]([CH:14]=1)[C:7]([O:9][C:10]([CH3:13])([CH3:12])[CH3:11])=[O:8]

참가 물질

4

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 10933837HCID 10933837, 화합물

생성물 1

HCID 66690636HCID 66690636, 화합물수율 91.5%

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
75 °C

실험 절차

To a solution of tert-butyl 5,6-dichloronicotinate (32.3 g, 130 mmol)) in ethanol (651 mL) was added hydrazine hydrate (19 mL, 391 mmol). The mixture was heated 75° C. After 2.5 h, the mixture was cooled to ambient temperature. The mixture was concentrated down to 200 mL of ethanol. The solid crashed out was filtered and washed with dichloromethane to give the hydrochloride salt of the title compound (29 g): LC-MS [M+1]=244.1.

후처리

  1. temperaturethe mixture was cooled to ambient temperature
  2. concentrationThe mixture was concentrated down to 200 mL of ethanol
  3. filtrationThe solid crashed out was filtered
  4. washwashed with dichloromethane

출처 및 근거

ORD 기록
ord-e8342a698cfb42e9bef38eb967d04cbd
출처 데이터셋
uspto-grants-2016_01
특허 번호
US09238647B2

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