Trimethyl orthoacetate → Methyl 5,6-Dichloronicotinate

HRID 217470

반응식

HRID 217470 반응식
[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]

참가 물질

4

반응물 2

HCID 15050Trimethyl orthoacetateHCID 2479875,6-Dichloronicotinic acid

생성물 1

HCID 2782166Methyl 5,6-Dichloronicotinate

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-8e51362fa5d44881a68264b9487a6ff4
출처 데이터셋
uspto-grants-2012_06
특허 번호
US08193378B2

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