Trimethyl orthoacetate → Methyl 5,6-Dichloronicotinate

HRID 217470

反応式

HRID 217470 の反応式
[Cl:1][C:2]1[C:3]([Cl:11])=[N:4][CH:5]=[C:6]([CH:10]=1)[C:7]([OH:9])=[O:8].[CH3:12]OC(OC)(OC)C>CCOC(C)=O>[Cl:1][C:2]1[C:3]([Cl:11])=[N:4][CH:5]=[C:6]([CH:10]=1)[C:7]([O:9][CH3:12])=[O:8]

参加物

4

反応物 2

HCID 15050Trimethyl orthoacetateHCID 2479875,6-Dichloronicotinic acid

生成物 1

HCID 2782166Methyl 5,6-Dichloronicotinate

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

To 5,6-dichloronicotinic acid (2.2 g) was added 1,1,1-trimethoxyethane (4.3 mL), followed by irradiation with microwave at 120° C. for 15 minutes. The reaction mixture was dissolved in EtOAc and washed with water. The organic layer was dried over MgSO4 and the vehicle was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (hexane:EtOAc=85:15 to 80:20) to obtain methyl 5,6-dichloronicotinate (2.2 g) as a white solid.

後処理

  1. customfollowed by irradiation with microwave at 120° C. for 15 minutes
  2. washwashed with water
  3. dry with materialThe organic layer was dried over MgSO4
  4. customthe vehicle was evaporated under reduced pressure
  5. customThe residue was purified by silica gel column chromatography (hexane:EtOAc=85:15 to 80:20)

出典と根拠

ORDレコード
ord-8e51362fa5d44881a68264b9487a6ff4
出典データセット
uspto-grants-2012_06
特許番号
US08193378B2

関連ノート

読み込み中…