Water → 4-n-Heptyl-4-phenyl-4-silacyclohexane carbaldehyde

HRID 2653

반응식

HRID 2653 반응식
C[C:2](C)([O-:4])C.[K+].[Cl-].COC[P+](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1.[CH2:30]([Si:37]1([C:44]2[CH:49]=[CH:48][CH:47]=[CH:46][CH:45]=2)[CH2:42][CH2:41][C:40](=O)[CH2:39][CH2:38]1)[CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][CH3:36].O>C1COCC1>[CH2:30]([Si:37]1([C:44]2[CH:49]=[CH:48][CH:47]=[CH:46][CH:45]=2)[CH2:42][CH2:41][CH:40]([CH:2]=[O:4])[CH2:39][CH2:38]1)[CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][CH3:36]

참가 물질

6

반응물 4

HCID 962WaterHCID 2723798Methoxymethyl-triphenylphosphonium chlorideHCID 195937974-n-Heptyl-4-phenyl-4-silacyclohexanoneHCID 23665647Potassium tert-butoxide

생성물 1

HCID 538308434-n-Heptyl-4-phenyl-4-silacyclohexane carbaldehyde

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

12 g of potassium t-butoxide was added to a mixture of 35 g of methoxymethyltriphenylphosphonium chloride and 200 ml of THF to prepare an orange ylide solution. A solution of 28 g of 4-n-heptyl-4-phenyl-4-silacyclohexanone in 50 ml of THF was added to the solution. After agitation for 2 hours at room temperature, the mixture was poured into iced water and extracted with methylene chloride. The extract was washed, dried and concentrated by a usual manner. n-Hexane was added to the resultant concentrate, followed by removal of the resultant triphenylphosphine oxide crystals by filtration. The resultant filtrate was concentrated. The concentrate was hydrolyzed with 100 ml of 20% hydrochloric acid, followed by washing, drying and concentration by a usual manner to obtain 4-n-heptyl-4-phenyl-4-silacyclohexane carbaldehyde.

후처리

  1. customto prepare an orange ylide solution
  2. extractionextracted with methylene chloride
  3. washThe extract was washed
  4. customdried
  5. concentrationconcentrated by a usual manner
  6. additionn-Hexane was added to the resultant
  7. concentrationconcentrate
  8. customfollowed by removal of the resultant triphenylphosphine oxide crystals by filtration
  9. concentrationThe resultant filtrate was concentrated
  10. washby washing
  11. customdrying
  12. concentrationconcentration by a usual manner

출처 및 근거

ORD 기록
ord-185154b6627f4f909d32b9149fae48a3
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05730901

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