Sodium Carbonate → 2-(3,5-Dimethyl-4-hydroxyphenyl)-2-(3,5-dimethyl-4-cyanatophenyl)-propane

HRID 1439533

反応式

HRID 1439533 の反応式
[CH3:1][C:2]1[CH:3]=[C:4]([C:10]([C:13]2[CH:18]=[C:17]([CH3:19])[C:16]([OH:20])=[C:15]([CH3:21])[CH:14]=2)([CH3:12])[CH3:11])[CH:5]=[C:6]([CH3:9])[C:7]=1[OH:8].[N:22]#[C:23]Cl.C([O-])([O-])=O.[Na+].[Na+]>O>[CH3:21][C:15]1[CH:14]=[C:13]([C:10]([C:4]2[CH:3]=[C:2]([CH3:1])[C:7]([O:8][C:23]#[N:22])=[C:6]([CH3:9])[CH:5]=2)([CH3:12])[CH3:11])[CH:18]=[C:17]([CH3:19])[C:16]=1[OH:20]

参加物

5

反応物 3

HCID 10340Sodium CarbonateHCID 10477Cyanogen ChlorideHCID 797174,4'-Isopropylidenedi-2,6-xylol

生成物 1

HCID 213958702-(3,5-Dimethyl-4-hydroxyphenyl)-2-(3,5-dimethyl-4-cyanatophenyl)-propane収率 99.5%

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

反応条件

温度
0 °C

実験手順

28.4 g (0.1 mol) of 2,2-bis-(3,5-dimethyl-4-hydroxyphenyl)-propane are suspended in 500 ml of water and 300 ml of dichloromethine. After cooling to 0° C, 15 ml (0.3 mol) of cyanogen chloride are added. 10.6 g (0.1 mol) of Na2CO3, dissolved in 50 ml of water, are then added dropwise over the course of 2 hours, with vigorous stirring, in such a way that a pH value of between 7.5 and 8.5 is maintained constantly in the reaction mixture. At the same time, the reaction temperature is kept at about 0° C by cooling. Thereafter, the reaction is terminated by slow addition of 1 N NaOH, the 1 N NaOH being added in such a way that a pH value of 7.5 to 8.0 is constantly maintained in the reaction mixture and persists as the final value. After the end of the reaction, the organic phase is separated off, washed with 50 ml of water and concentrated at room temperature. 30.8 g (99% of theory) of 2-(3,5-dimethyl-4-hydroxyphenyl)-2-(3,5-dimethyl-4-cyanatophenyl)-propane are obtained as the residue.

後処理

  1. additionare then added dropwise over the course of 2 hours, with vigorous stirring
  2. temperaturein such a way that a pH value of between 7.5 and 8.5 is maintained constantly in the reaction mixture
  3. customis kept at about 0° C
  4. temperatureby cooling
  5. customThereafter, the reaction is terminated by slow addition of 1 N NaOH
  6. additionthe 1 N NaOH being added in such a way that a pH value of 7.5 to 8.0
  7. temperatureis constantly maintained in the reaction mixture and persists as the final value
  8. customAfter the end of the reaction
  9. customthe organic phase is separated off
  10. washwashed with 50 ml of water
  11. concentrationconcentrated at room temperature

出典と根拠

ORDレコード
ord-7c8f2af6766d48b5a25ab45950dde1c7
出典データセット
uspto-grants-1977_11
特許番号
US04060541

関連ノート

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