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

HRID 2171224ノート

反応式

HRID 2171224 の反応式
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]

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-e96574f100e948fc8f2c384cb915ea24
出典データセット
uspto-grants-2015_06
特許番号
US09051310B2

反応ノート

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