Cyanogen Bromide → HCID 13881444、化合物

HRID 894580ノート

反応式

HRID 894580 の反応式
[CH3:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([CH3:8])[C:3]=1[NH:9][CH2:10][CH2:11][NH:12][C:13]1[C:18]([CH3:19])=[CH:17][CH:16]=[CH:15][C:14]=1[CH3:20].[N:21]#[C:22][Br:23]>C1(C)C(C)=CC=CC=1>[BrH:23].[CH3:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([CH3:8])[C:3]=1[N:9]1[CH2:10][CH2:11][N:12]([C:13]2[C:18]([CH3:19])=[CH:17][CH:16]=[CH:15][C:14]=2[CH3:20])[C:22]1=[NH:21]

参加物

4

反応物 2

HCID 10476Cyanogen BromideHCID 3931947STK753189

生成物 1

HCID 13881444HCID 13881444、化合物収率 99.4%

試薬・触媒・溶媒 1

HCID 7237O-Xylene溶媒3 回

実験手順

500 ml of xylene are introduced into 1 liter four-necked flask equipped with a stirrer, reflux condenser, thermometer and dropping funnel of 100 ml capacity. 72.5 g (0.27 moles) of 1,2-bis(2',6'-dimethylphenyl-amino)-ethane are dissolved in the xylene, and a solution of 33.9 g (0.32 moles) of cyanogen bromide in 200 ml of xylene is added dropwise, within about 1.5 hours, to the stirred solution at an internal temperature of 110° to 115° C. After the addition the mixture is stirred for a further hour at 110° to 115° C. and then it is allowed to cool. The separated precipitate is filtered off, washed with xylene and diethyl ether, and dried at room temperature. 100.5 g (99.4%) of 1,3-bis(2',6'-dimethylphenyl)-2-imino-imidazolidine hydrobromide are obtained as colourless crystals melting at 289°-290° C.

後処理

  1. customequipped with a stirrer
  2. temperaturereflux condenser
  3. additionAfter the addition the mixture
  4. temperatureto cool
  5. filtrationThe separated precipitate is filtered off
  6. washwashed with xylene and diethyl ether
  7. customdried at room temperature

出典と根拠

ORDレコード
ord-24ede272932c465fbc3e1869daf58931
出典データセット
uspto-grants-1981_08
特許番号
US04284642

反応ノート

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