Hydrochloric Acid → HCID 178440085、化合物

HRID 265170

反応式

HRID 265170 の反応式
O.[OH-].[Li+].[OH:4][C:5]([C:8]1[N:9]=[C:10]([CH2:18][CH2:19][CH3:20])[NH:11][C:12]=1[C:13]([O:15]CC)=[O:14])([CH3:7])[CH3:6].Cl>O.CO>[OH:4][C:5]([C:8]1[N:9]=[C:10]([CH2:18][CH2:19][CH3:20])[NH:11][C:12]=1[C:13]([OH:15])=[O:14])([CH3:7])[CH3:6]

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 168937Lithium hydroxide, monohydrateHCID 178440079HCID 178440079、化合物

生成物 1

HCID 178440085HCID 178440085、化合物収率 47.2%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

A solution of 0.28 g of lithium hydroxide monohydrate in 5 ml of water was added to a solution of 0.48 g of ethyl 4-(1-hydroxy-1-methylethyl)-2-propylimidazole-5-carboxylate (prepared as described in Preparation 9) in 5 ml of methanol, and the resulting mixture was stirred at room temperature for 18 hours. At the end of this time, the pH of the reaction mixture was adjusted to a value of 2.3 by adding 6.67 ml of 1N aqueous hydrochloric acid, and the mixture was concentrated by evaporation under reduced pressure to a volume of about 2 ml. The crystals which precipitated were collected by filtration to give 0.20 g of the title compound, melting at 232° C. (with decomposition).

後処理

  1. concentrationthe mixture was concentrated by evaporation under reduced pressure to a volume of about 2 ml
  2. customThe crystals which precipitated
  3. filtrationwere collected by filtration

出典と根拠

ORDレコード
ord-68f74b739147478da33b88b5e222870b
出典データセット
uspto-grants-1997_07
特許番号
US05646171

関連ノート

読み込み中…