2,4-Dichlorobenzyl chloride → 2,4-Dichlorobenzyl alcohol

HRID 2058553

反応式

HRID 2058553 の反応式
[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[CH3:9].Cl[CH2:11][C:12]1[CH:17]=[CH:16][C:15]([Cl:18])=[CH:14][C:13]=1[Cl:19].ClC(Cl)[C:22]1[CH:27]=[CH:26][C:25]([Cl:28])=[CH:24][C:23]=1[Cl:29].[C:31](=[O:34])(O)[O-:32].[Na+]>O>[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[CH3:9].[Cl:19][C:13]1[CH:14]=[C:15]([Cl:18])[CH:16]=[CH:17][C:12]=1[CH:11]=[O:32].[Cl:28][C:25]1[CH:24]=[C:23]([Cl:29])[CH:22]=[CH:27][C:26]=1[CH2:31][OH:34]

参加物

8

反応物 4

HCID 72122,4-Dichlorobenzyl chlorideHCID 72542,4-DichlorotolueneHCID 86372,4-Dichloro-1-(dichloromethyl)benzeneHCID 516892Sodium Bicarbonate

生成物 3

HCID 72542,4-Dichlorotoluene収率 11.84%HCID 134042,4-Dichlorobenzaldehyde収率 16.94%HCID 156842,4-Dichlorobenzyl alcohol収率 71.21%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
160 °C

実験手順

To a 600 cc Hastoloy C autoclave was charged 48.52 g of a crude chlorination mixture containing 10.93% 2,4-dichlorotoluene, 70.39% α,2,4-trichlorotoluene, 18.52% α,α,2,4-tetrachlorotoluene, 0.10% α,α,2,4-pentachlorotoluene (the percentages represent gas chromatograph area percents), 39 g of sodium bicarbonate and 146 ml of water. The autoclave was flushed with nitrogen and pressure tested to 1500 psig. The autoclave was then vented to atmospheric pressure and heated. The temperature was increased to 160° C. and maintained for two hours. The pressure increased from atmosphere pressure to between 200 and 400 psig. After two hours, the autoclave was cooled to 80° C., vented and the product removed. After separation of the aqueous phase, the crude aldehyde mixture was flash distilled affording 11.84% 2,4-dichlorotoluene, 16.94% 2,4-dichlorobenzaldehyde and 71.21% 2,4-dichlorobenzyl alcohol.

後処理

  1. additionTo a 600 cc Hastoloy C autoclave was charged 48.52 g of a crude chlorination mixture
  2. customThe autoclave was flushed with nitrogen and pressure
  3. temperatureheated
  4. temperaturemaintained for two hours
  5. temperatureThe pressure increased from atmosphere pressure to between 200 and 400 psig
  6. temperaturethe autoclave was cooled to 80° C.
  7. customthe product removed
  8. customAfter separation of the aqueous phase
  9. distillationdistilled

出典と根拠

ORDレコード
ord-08541278214043bc831c91b6bc57fb60
出典データセット
uspto-grants-1982_03
特許番号
US04317934

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