Potassium Hydroxide → HCID 178524321、化合物

HRID 368328ノート

反応式

HRID 368328 の反応式
Cl.[NH:2]1[CH:6]=[C:5]([CH2:7][CH2:8][O:9][C:10]2[CH:11]=[C:12]3[C:17](=[CH:18][CH:19]=2)[C:16](=[O:20])[CH2:15][CH2:14][CH2:13]3)[N:4]=[CH:3]1.C([CH2:24][C:25]1[S:29][C:28]([CH:30]=[O:31])=[CH:27][CH:26]=1)(O)=O.[OH-:32].[K+]>CCO>[NH:2]1[CH:6]=[C:5]([CH2:7][CH2:8][O:9][C:10]2[CH:11]=[C:12]3[C:17](=[CH:18][CH:19]=2)[C:16](=[O:20])[C:15](=[CH:24][C:25]2[S:29][C:28]([C:30]([OH:31])=[O:32])=[CH:27][CH:26]=2)[CH2:14][CH2:13]3)[N:4]=[CH:3]1

参加物

5

反応物 3

HCID 14797Potassium HydroxideHCID 186265125-Carboxymethyl-2-thiophene carboxaldehydeHCID 178479625HCID 178479625、化合物

生成物 1

HCID 178524321HCID 178524321、化合物収率 75%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

According to the method of Example 34, 6-[2-(1H-imidazole-4-yl)-ethoxy]-3,4-dihydro-2H-naphthalen-1-one, monohydrochloride (0.220 g, 0.75 mmol) was reacted with 5-carboxymethyl-2-thiophene carboxaldehyde (0.191 g, 1.12 mmol) in 5 mL of 4% KOH in EtOH overnight, and the resulting solid was purified by preparative HPLC (C18, 0.1% TFA in H2O:0.1% TFA in AcCN; gradient 80:20 to 20:80) to afford 0.302 g (75%) of the title compound as a light tan powder, mp dec. >200° C.: APCI-MS m/e 395 (M+ +1).

後処理

  1. customthe resulting solid was purified by preparative HPLC (C18, 0.1% TFA in H2O:0.1% TFA in AcCN; gradient 80:20 to 20:80)

出典と根拠

ORDレコード
ord-40a70ce756b24e629ec6ba5cebc1361a
出典データセット
uspto-grants-2000_10
特許番号
US06133303

反応ノート

読み込み中…