HCID 14835675、化合物 → HCID 14835676、化合物

反応式

[CH3:1][O:2][CH:3]([O:14][CH3:15])[C:4]1[CH:5]=[C:6]([CH:11]=[CH:12][CH:13]=1)[C:7]([NH:9][NH2:10])=[O:8].[CH:16]([O-])([O-])OC>>[CH3:15][O:14][CH:3]([O:2][CH3:1])[C:4]1[CH:5]=[C:6]([C:7]2[O:8][CH:16]=[N:10][N:9]=2)[CH:11]=[CH:12][CH:13]=1

参加物

反応物 2

HCID 14835675HCID 14835675、化合物

HCID 53629101Methylorthoformate

生成物 1

HCID 14835676HCID 14835676、化合物収率 61.4%

実験手順

2.1 g of 3-dimethoxymethylbenzhydrazide and 12.7 g of methyl orthoformate were reacted at atmospheric pressure for 24 hours while distilling off the methanol formed. Excessive methyl orthoformate was removed by distillation under reduced pressure. The residue was purified by a column chromatography (eluant: n-hexane/ethyl acetate=3/1) to obtain 1.35 g of colorless oily 2-(3-dimethoxymethylphenyl)-1,3,4-oxadiazole.

後処理

distillationwhile distilling off the methanol
customformed
customExcessive methyl orthoformate was removed by distillation under reduced pressure
customThe residue was purified by a column chromatography (eluant: n-hexane/ethyl acetate=3/1)

出典と根拠

ORDレコード: ord-4d560382b83a44feb0a329157b3c91ab
出典データセット: uspto-grants-1990_08
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US04948796

反応ノート

読み込み中…

参加物