Hydrazine hydrate (1:1) → HCID 66690636、化合物

HRID 592296ノート

反応式

HRID 592296 の反応式
[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]

参加物

4

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 10933837HCID 10933837、化合物

生成物 1

HCID 66690636HCID 66690636、化合物収率 91.5%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
75 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-e8342a698cfb42e9bef38eb967d04cbd
出典データセット
uspto-grants-2016_01
特許番号
US09238647B2

反応ノート

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