Gamma-Butyrolactone → HCID 178520699、化合物

反応式

[O:1]([C@H:5]1[CH2:10][CH2:9][C@H:8]([NH2:11])[CH2:7][CH2:6]1)[N+:2]([O-:4])=[O:3].[C:12]1(=[O:17])[O:16][CH2:15][CH2:14][CH2:13]1>>[OH:17][CH2:12][CH2:13][CH2:14][C:15]([NH:11][C@H:8]1[CH2:7][CH2:6][C@H:5]([O:1][N+:2]([O-:4])=[O:3])[CH2:10][CH2:9]1)=[O:16]

参加物

反応物 2

HCID 7302Gamma-Butyrolactone

HCID 178511725HCID 178511725、化合物

生成物 1

HCID 178520699HCID 178520699、化合物

実験手順

4.8 g (0.03 mol) trans-4-nitroxycyclohexylamine are mixed with 5.7 ml 4-butyrolactone and stirred for 3 d at room temperature. For the removal of the excess lactone, it is filtered over a silicic gel acid with ethyl acetate. After collection of the pure fractions, it is distilled in a vacuum, triturated with ether and filtered off with suction. There remain 2.1 g of the title compound of the melting point 58°-60° C., i.e. 28% of theory.

後処理

customFor the removal of the excess lactone, it
filtrationis filtered over a silicic gel acid with ethyl acetate
customAfter collection of the pure fractions, it
distillationis distilled in a vacuum
customtriturated with ether
filtrationfiltered off with suction

出典と根拠

ORDレコード: ord-804ea5da64ca4972b7c3a4735b112a1e
出典データセット: uspto-grants-1995_05
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US05411989

反応ノート

読み込み中…

参加物