Triethylamine → 1,4-Bis(4-chloro-3-nitrophenyl)butane-1,4-diyl dimethanesulfonate

HRID 1470924ノート

反応式

HRID 1470924 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([OH:23])[CH2:9][CH2:10][CH:11]([C:13]2[CH:18]=[CH:17][C:16]([Cl:19])=[C:15]([N+:20]([O-:22])=[O:21])[CH:14]=2)[OH:12])=[CH:4][C:3]=1[N+:24]([O-:26])=[O:25].C(N(CC)CC)C.[CH3:34][S:35](Cl)(=[O:37])=[O:36]>ClCCl>[CH3:34][S:35]([O:12][CH:11]([C:13]1[CH:18]=[CH:17][C:16]([Cl:19])=[C:15]([N+:20]([O-:22])=[O:21])[CH:14]=1)[CH2:10][CH2:9][CH:8]([O:23][S:35]([CH3:34])(=[O:37])=[O:36])[C:5]1[CH:6]=[CH:7][C:2]([Cl:1])=[C:3]([N+:24]([O-:26])=[O:25])[CH:4]=1)(=[O:37])=[O:36]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 767088951,4-Bis(4-chloro-3-nitrophenyl)butane-1,4-diol

生成物 1

HCID 767087941,4-Bis(4-chloro-3-nitrophenyl)butane-1,4-diyl dimethanesulfonate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

The product of Example 28B (4.81 g, 11.99 mmol) and triethylamine (5.85 mL, 42.0 mmol) were dissolved in dichloromethane (80 mL) at room temperature and treated with methanesulfonyl chloride (2.34 mL, 30.0 mmol) dropwise over 10 minutes. The resulting solution was stirred for 2 h then concentrated to dryness and used directly in the next step.

後処理

  1. concentrationthen concentrated to dryness

出典と根拠

ORDレコード
ord-52f291a38f054179a5a611d7af64ff58
出典データセット
uspto-grants-2015_04
特許番号
US09006387B2

反応ノート

読み込み中…