Water → HCID 59133000、化合物

HRID 2241795ノート

反応式

HRID 2241795 の反応式
[Cl-].[CH3:2][O:3][CH2:4][P+](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1.CC(C)([O-])C.[K+].[CH:30]1([CH:37]2[CH2:42][CH2:41][C:40](=O)[CH2:39][CH2:38]2)[CH2:35][CH2:34][C:33](=O)[CH2:32][CH2:31]1.O.C1[CH2:49][O:48][CH2:47]C1>>[CH3:2][O:3][CH:4]=[C:33]1[CH2:34][CH2:35][CH:30]([CH:37]2[CH2:42][CH2:41][C:40](=[CH:47][O:48][CH3:49])[CH2:39][CH2:38]2)[CH2:31][CH2:32]1

参加物

6

反応物 5

HCID 962WaterHCID 8028Tetrahydrofuran2 回HCID 264825(1,1'-Bicyclohexyl)-4,4'-dioneHCID 2723798Methoxymethyl-triphenylphosphonium chlorideHCID 23665647Potassium tert-butoxide

生成物 1

HCID 59133000HCID 59133000、化合物

反応条件

温度
-10 °C

実験手順

882.3 g of methoxymethyltriphenylphosphonium chloride was dispersed in 2,600 mL of THF, followed by cooling to −10° C. 313.2 g of potassium-t-butoxide were added while maintaining the inner temperature. After stirring or one hours, a THF (800 mL) solution of 200.0 g of bicyclohexyl-4,4′-dione was and added dropwise. After stirring for 1 hour while maintaining the inner temperature, water was added thereby terminating the reaction. The solvent was distilled off under reduced pressure and hexane was added, followed by stirring and vigorous stirring and further filtration (twice). The filtrates were combined, washed in turn with an aqueous 50% methanol solution and saturated saline, and then dried over anhydrous magnesium sulfate. The solvent was distilled off to obtain 231.8 g of a white solid.

後処理

  1. temperaturewhile maintaining the inner temperature
  2. additionadded dropwise
  3. stirringAfter stirring for 1 hour
  4. additionwas added
  5. customthereby terminating
  6. customthe reaction
  7. distillationThe solvent was distilled off under reduced pressure and hexane
  8. additionwas added
  9. stirringby stirring
  10. stirringvigorous stirring
  11. filtrationfurther filtration (twice)
  12. washwashed in turn with an aqueous 50% methanol solution and saturated saline
  13. dry with materialdried over anhydrous magnesium sulfate
  14. distillationThe solvent was distilled off

出典と根拠

ORDレコード
ord-4ee55c6b5ab54a33a9ebaaaf8213b068
出典データセット
uspto-grants-2010_03
特許番号
US07670504B2

反応ノート

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