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Hydrochloric Acid → 6-(2-Chloroethyl)-1,3,3-trimethylbicyclo[2.2.2]octan-2-one

HRID 441587
ノート
印刷プレビュー

反応式

HRID 441587 の反応式
[CH3:1][C:2]12[CH2:12][CH2:11][CH:5]([CH2:6][CH:7]1[CH2:8][CH2:9]O)[C:4]([CH3:14])([CH3:13])[C:3]2=[O:15].S(Cl)([Cl:18])=O.Cl>C1C=CC=CC=1>[CH3:1][C:2]12[CH2:12][CH2:11][CH:5]([CH2:6][CH:7]1[CH2:8][CH2:9][Cl:18])[C:4]([CH3:14])([CH3:13])[C:3]2=[O:15]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 24386Thionyl Chloride3 回HCID 21419393HCID 21419393、化合物

生成物 1

HCID 213335696-(2-Chloroethyl)-1,3,3-trimethylbicyclo[2.2.2]octan-2-one

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

反応条件

温度
90 °C

実験手順

To a 100 ml microflask equipped with thermometer, reflux condenser, dropping funnel and magnetic stirrer is charged 12.3 g of 1,3,3-trimethyl-6-(2-hydroxyethyl)bicyclo(2.2.2)-octan-2-one prepared according to the process of Example XVII, and 20 ml benzene. The dropping funnel is charged with 12 g thionyl chloride. The thionyl chloride is added to the reaction mass from the dropping funnel, slowly, over a period of five minutes as the temperature of the reaction mass rises to 35° C. The reaction mass is then refluxed for a period of 10 hours at 90° C. The flask is then vented to the atmosphere and heated on a steam bath in order to volatilize the unreacted thionyl chloride and any hydrogen chloride reaction product remaining. The reaction mass is then cooled and hydrolyzed with 50 g ice. The organic layer is separated, and the aqueous phase is extracted with four 20 ml portions of anhydrous diethyl ether. The organic layers are bulked and washed with (i) three 20 ml portions of saturated sodium bicarbonate solution and (ii) one 20 ml portion of water. The organic phase is then dried over anhydrous magnesium sulfate and stripped of the diethyl ether. The reaction product is then distilled at 105°-115° C. at a pressure of 0.2 mm Hg. Its structure, confirmed by NMR and mass spectral analyses is as follows: ##STR37##

後処理

  1. customTo a 100 ml microflask equipped with thermometer
  2. temperaturereflux condenser
  3. customprepared
  4. temperatureheated on a steam bath in order
  5. customThe organic layer is separated
  6. extractionthe aqueous phase is extracted with four 20 ml portions of anhydrous diethyl ether
  7. washwashed with (i) three 20 ml portions of saturated sodium bicarbonate solution and (ii) one 20 ml portion of water
  8. dry with materialThe organic phase is then dried over anhydrous magnesium sulfate
  9. distillationThe reaction product is then distilled at 105°-115° C. at a pressure of 0.2 mm Hg

出典と根拠

ORDレコード
ord-823d3e2efdd442f8b1becc577367877d
出典データセット
uspto-grants-1977_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04041084

反応ノート

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