Ethylamine → HCID 67223854、化合物

反応式

CO[C:3](=[O:15])[C:4]1[CH:9]=[CH:8][C:7]([N+:10]([O-:12])=[O:11])=[CH:6][C:5]=1[CH2:13]Br.[CH2:16]([NH2:18])[CH3:17]>>[CH2:16]([N:18]1[CH2:13][C:5]2[C:4](=[CH:9][CH:8]=[C:7]([N+:10]([O-:12])=[O:11])[CH:6]=2)[C:3]1=[O:15])[CH3:17]

参加物

反応物 2

HCID 6341Ethylamine

HCID 15088701Methyl 2-(bromomethyl)-4-nitrobenzoate

生成物 1

HCID 67223854HCID 67223854、化合物収率 85%

実験手順

2-Bromomethyl-4-nitro-benzoic acid methyl ester (1.0 g, 3.64 mmol) was stirred in ethylamine (30 ml, 2.0M solution in THF) at room temperature. The reaction was stirred for 3 hrs, after which time the solvent was evaporated in vacuo and the crude residue triturated with diethyl ether. The resulting orange solid was filtered and dried in a vacuum oven (40° C.) to afford the title compound (634 mg, 85%). HPLC retention time 3.56 min. Mass spectrum (ES+) m/z 207 (M+H).

後処理

customafter which time the solvent was evaporated in vacuo
customthe crude residue triturated with diethyl ether
filtrationThe resulting orange solid was filtered
customdried in a vacuum oven (40° C.)

出典と根拠

ORDレコード: ord-5ad813b72e9c4db48b1d82d0f7da6752
出典データセット: uspto-grants-2013_03
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US08399481B2

反応ノート

読み込み中…

参加物