Sodium Carbonate → 1-(4-Hydroxyphenyl)-1-(4-cyanatophenyl)-cyclohexane

HRID 1439535

반응식

HRID 1439535 반응식
[OH:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2([C:14]3[CH:19]=[CH:18][C:17]([OH:20])=[CH:16][CH:15]=3)[CH2:13][CH2:12][CH2:11][CH2:10][CH2:9]2)=[CH:4][CH:3]=1.[N:21]#[C:22]Cl.C([O-])([O-])=O.[Na+].[Na+].[OH-].[Na+]>O.C(Cl)Cl>[OH:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2([C:14]3[CH:15]=[CH:16][C:17]([O:20][C:22]#[N:21])=[CH:18][CH:19]=3)[CH2:9][CH2:10][CH2:11][CH2:12][CH2:13]2)=[CH:6][CH:7]=1

참가 물질

7

반응물 4

HCID 10340Sodium CarbonateHCID 10477Cyanogen ChlorideHCID 14798Sodium HydroxideHCID 2324461,1-Bis(4-hydroxyphenyl)cyclohexane

생성물 1

HCID 213958671-(4-Hydroxyphenyl)-1-(4-cyanatophenyl)-cyclohexane수율 99%

시약·촉매·용매 2

HCID 962Water용매2회HCID 6344Dichloromethane용매

실험 절차

86.8 g (0.1 mol) of 1,1-bis-(4-hydroxyphenyl)-cyclo hexane are suspended in 500 ml of water and 300 ml of methylene chloride at about 0° to 3° C. 20 ml (0.4 mol) of cyanogen chloride are added to this suspension and a solution of 10.6 g (0.1 mol) of Na2CO3 in 50 ml of water is added dropwise over the course of 90 minutes at the same temperature, with vigorous stirring, in such a way that a pH value between 7.5 and 8.5 is maintained in the reaction mixture. Thereafter, 1 N NaOH is added at 0° C in such a way that the abovementioned pH value is maintained, and persists as the final value. Thereafter, the organic phase is separated off and washed with 50 ml of water and the solvent is stripped off at room temperature. 29 g (99% of theory) of 1-(4-hydroxyphenyl)-1-(4-cyanatophenyl)-cyclohexane are thus obtained.

후처리

  1. customat about 0° to 3° C
  2. temperaturein such a way that a pH value between 7.5 and 8.5 is maintained in the reaction mixture
  3. temperatureis maintained
  4. customThereafter, the organic phase is separated off
  5. washwashed with 50 ml of water
  6. customis stripped off at room temperature

출처 및 근거

ORD 기록
ord-2448ea548d0c4864876da647f0934506
출처 데이터셋
uspto-grants-1977_11
특허 번호
US04060541

연결된 노트

불러오는 중…