Dimethylformamide → Methyl 2,3-difluoro-5-nitrobenzoate

HRID 2171224노트

반응식

HRID 2171224 반응식
C(Cl)(=O)C(Cl)=O.CN([CH:10]=[O:11])C.C(Cl)Cl.[F:15][C:16]1[C:24]([F:25])=[CH:23][C:22]([N+:26]([O-:28])=[O:27])=[CH:21][C:17]=1[C:18](O)=[O:19]>CO>[F:15][C:16]1[C:24]([F:25])=[CH:23][C:22]([N+:26]([O-:28])=[O:27])=[CH:21][C:17]=1[C:18]([O:11][CH3:10])=[O:19]

참가 물질

6

반응물 4

HCID 6228DimethylformamideHCID 6344DichloromethaneHCID 65578Oxalyl chlorideHCID 545937902,3-Difluoro-5-nitrobenzoic acid

생성물 1

HCID 62662214Methyl 2,3-difluoro-5-nitrobenzoate

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

Oxalyl chloride (1 ml) and DMF (5 μl) were added to a CH2Cl2 (1.6 ml) solution containing 2,3-difluoro-5-nitrobenzoic acid (1.61 g) obtained in the 1st step, followed by stirring at room temperature for 15 minutes. The reaction solution was poured into a liquid mixture of MeOH/Py (100 ml/1.28 ml) and the solvent was distilled away under reduced pressure. The obtained residue was purified by silica gel chromatography (n-hexane:ethyl acetate=1:0 to 4:1). A light yellow solid of methyl 2,3-difluoro-5-nitrobenzoate (1.71 g) was thus obtained.

후처리

  1. customobtained in the 1st step
  2. distillationthe solvent was distilled away under reduced pressure
  3. customThe obtained residue was purified by silica gel chromatography (n-hexane:ethyl acetate=1:0 to 4:1)

출처 및 근거

ORD 기록
ord-e96574f100e948fc8f2c384cb915ea24
출처 데이터셋
uspto-grants-2015_06
특허 번호
US09051310B2

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