Cyanogen Bromide → HCID 13881444, 화합물

HRID 894580노트

반응식

HRID 894580 반응식
[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]

참가 물질

4

반응물 2

HCID 10476Cyanogen BromideHCID 3931947STK753189

생성물 1

HCID 13881444HCID 13881444, 화합물수율 99.4%

시약·촉매·용매 1

HCID 7237O-Xylene용매3회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-24ede272932c465fbc3e1869daf58931
출처 데이터셋
uspto-grants-1981_08
특허 번호
US04284642

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