Hydrazine hydrate (1:1) → 6-Chloro-imidazo[1,2-b]pyridazine-8-carboxylic acid hydrazide

HRID 1969104ノート

反応式

HRID 1969104 の反応式
C([O:3][C:4]([C:6]1[C:7]2[N:8]([CH:13]=[CH:14][N:15]=2)[N:9]=[C:10]([Cl:12])[CH:11]=1)=O)C.O.[NH2:17][NH2:18]>C(O)C>[Cl:12][C:10]1[CH:11]=[C:6]([C:4]([NH:17][NH2:18])=[O:3])[C:7]2[N:8]([CH:13]=[CH:14][N:15]=2)[N:9]=1

参加物

4

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 57786728Ethyl 6-chloroimidazo[1,2-b]pyridazine-8-carboxylate

生成物 1

HCID 577866686-Chloro-imidazo[1,2-b]pyridazine-8-carboxylic acid hydrazide収率 57%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a solution of crude 6-chloro-imidazo[1,2-b]pyridazine-8-carboxylic acid ethyl ester (5.00 g, “22 mmol”) in 40 mL of ethanol at 0-5° C. was added 10 mL of hydrazine hydrate. Yellow solid immediately precipitated. After 15 min. at 0-5° C., the solid was isolated by Buchner filtration, rinsing well with ice-cold ethanol (250 mL total) and dried by sucking air through then in vacuo. A small amount of additional solid precipated from the filtrate and was isolated and dried similarly to the first crop. A total of 2.38 g (57% over three steps) of 6-chloro-imidazo[1,2-b]pyridazine-8-carboxylic acid hydrazide was isolated as a yellow solid.

後処理

  1. customYellow solid immediately precipitated
  2. customthe solid was isolated by Buchner filtration
  3. washrinsing well with ice-cold ethanol (250 mL total)
  4. customdried
  5. customA small amount of additional solid precipated from the filtrate and was isolated
  6. customdried similarly to the first crop

出典と根拠

ORDレコード
ord-7768b1badc6d42ada02d6eae700bea02
出典データセット
uspto-grants-2013_04
特許番号
US08426441B2

反応ノート

読み込み中…