Triethylamine → Methyl 6-chloro-4-hydrazinonicotinate

HRID 588078

反応式

HRID 588078 の反応式
Cl[C:2]1[CH:7]=[C:6]([Cl:8])[N:5]=[CH:4][C:3]=1[C:9]([O:11][CH3:12])=[O:10].C(N(CC)CC)C.[NH2:20][NH2:21].O>C(O)C>[Cl:8][C:6]1[CH:7]=[C:2]([NH:20][NH2:21])[C:3]([C:9]([O:11][CH3:12])=[O:10])=[CH:4][N:5]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 24654Hydrazine hydrate (1:1)HCID 2764083Methyl4,6-dichloronicotinate

生成物 1

HCID 45588417Methyl 6-chloro-4-hydrazinonicotinate

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

Into a 20-L 4-necked round-bottom flask was placed methyl 4,6-dichloropyridine-3-carboxylate (1200 g, 5.82 mol), ethanol (10 L), and triethylamine (1182 g, 11.68 mol). NH2NH2.H2O (351 g, 7.02 mol) was then added drop-wise to the reaction mixture at 0° C. The resulting solution was heated to reflux for 1 h. The reaction mixture was cooled to room temperature. The solid was collected by filtration to give methyl 6-chloro-4-hydrazinylnicotinate, which was carried onto the next step without further purification.

後処理

  1. customInto a 20-L 4-necked round-bottom flask was placed
  2. temperatureThe resulting solution was heated
  3. temperatureto reflux for 1 h
  4. filtrationThe solid was collected by filtration

出典と根拠

ORDレコード
ord-f14e0ca123864c9ba7052da4033393ae
出典データセット
uspto-grants-2016_01
特許番号
US09226922B2

関連ノート

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