Ammonium Hydroxide → HCID 21432968、化合物

反応式

[OH-].[NH4+:2].C[O:4][C:5]([C:7]1[CH:12]=[C:11]([Br:13])[C:10]([OH:14])=[C:9]([Br:15])[N:8]=1)=O>>[Br:13][C:11]1[C:10]([OH:14])=[C:9]([Br:15])[N:8]=[C:7]([C:5]([NH2:2])=[O:4])[CH:12]=1

参加物

反応物 2

HCID 14923Ammonium Hydroxide

HCID 20674264HCID 20674264、化合物

生成物 1

HCID 21432968HCID 21432968、化合物収率 80%

実験手順

Concentrated ammonium hydroxide, 180 ml, was added to 10 g of 4,6-dibromo-5-hydroxy-2-pyridinecarboxylic acid methyl ester and heated at 45°-60° C. for 1 hour. After the mixture was kept for 2 days at room temperature, the solid was filtered and successively washed with dilute HCl (to neutralize the ammonia) and then with methanol and benzene to remove any unreacted starting material. The product was isolated in 80% yield; m.p. 261-266° C. (best sample: m.p. 275° C.).

後処理

temperatureheated at 45°-60° C. for 1 hour
filtrationthe solid was filtered
washsuccessively washed with dilute HCl (
customto remove
customThe product was isolated in 80% yield

出典と根拠

ORDレコード: ord-2500c11cac2b4ba094224738a5d04dfc
出典データセット: uspto-grants-1977_05
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US04025333

反応ノート

読み込み中…

参加物