Bis(2-chloroethyl)amine hydrochloride → HCID 178515209、化合物

HRID 252944ノート

反応式

HRID 252944 の反応式
[NH2:1][C:2]1[CH:11]=[CH:10][C:9]2[NH:8][CH:7]=[C:6]3[C:12](=[O:21])[N:13]([C:15]4[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=4)[N:14]=[C:5]3[C:4]=2[CH:3]=1.Cl.Cl[CH2:24][CH2:25][NH:26][CH2:27][CH2:28]Cl>ClC1C=CC=CC=1>[C:15]1([N:13]2[C:12](=[O:21])[C:6]3=[CH:7][NH:8][C:9]4[CH:10]=[CH:11][C:2]([N:1]5[CH2:28][CH2:27][NH:26][CH2:25][CH2:24]5)=[CH:3][C:4]=4[C:5]3=[N:14]2)[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1

参加物

4

反応物 2

HCID 522769Bis(2-chloroethyl)amine hydrochlorideHCID 178507347HCID 178507347、化合物

生成物 1

HCID 178515209HCID 178515209、化合物収率 75%

試薬・触媒・溶媒 1

HCID 7964Chlorobenzene溶媒

反応条件

温度
175 °C

実験手順

Equimolar quantities of 6a and bis(chloroethyl)amine hydrochloride were suspended in chlorobenzene and stirred at 175° C. for 60 hours. The solid was collected by filtration and washed with methanol, acetonitrile and diethylether in 75% yield. 1H-NMR (DMSO-d6) δ (ppm): 3.25 (4H, br), 3.52 (4H, br), 7.12 (1H, t, J=7.47 Hz), 7.39 (3H, m), 7.45 (1H, m), 7.68 (1H, m), 8.22 (2H, dd, J=8.55, 0.98 Hz), 8.60 (1H, d, J=5.86 Hz), 9.12 (1H, br). m/z 346.4 (MH+).

後処理

  1. filtrationThe solid was collected by filtration
  2. washwashed with methanol, acetonitrile and diethylether in 75% yield

出典と根拠

ORDレコード
ord-ab89ad9089c04212b6895f153616f387
出典データセット
uspto-grants-2011_01
特許番号
US07872002B2

反応ノート

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