Water → HCID 59133000, 화합물

HRID 1674431노트

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HRID 1674431 반응식
[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

참가 물질

6

반응물 5

HCID 962WaterHCID 8028Tetrahydrofuran2회HCID 264825(1,1'-Bicyclohexyl)-4,4'-dioneHCID 2723798Methoxymethyl-triphenylphosphonium chlorideHCID 23665647Potassium tert-butoxide

생성물 1

HCID 59133000HCID 59133000, 화합물

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온도
-10 °C

실험 절차

882.3 g of methoxymethyl triphenylphosphonium chloride was dispersed in 2600 mL of THF, and was cooled to −10° C. While keeping the internal temperature, 313.2 g of potassium-t-butoxide was added thereto. While keeping the internal temperature, the solution was stirred for 1 hour, and then THF (800 mL) solution containing 200.0 g of bicyclohexyl-4,4′-dione was added dropwise. While keeping the internal temperature, the solution was stirred for 1 hour, and then water was added to stop the reaction. The solvent was evaporated under reduced pressure. Then, the residue was added with hexane, was vigorously stirred, and was subjected to filtration (twice). The resultant product was mixed with the filtrate, then washed with 50% methanol aqueous solution and saturated saline in this order, and dried over anhydrous magnesium sulfate. The solvent was evaporated, to obtain 231.8 g of a white solid.

후처리

  1. additionwas added
  2. additionwas added dropwise
  3. stirringthe solution was stirred for 1 hour
  4. customthe reaction
  5. customThe solvent was evaporated under reduced pressure
  6. additionThen, the residue was added with hexane
  7. stirringwas vigorously stirred
  8. filtrationwas subjected to filtration (twice)
  9. additionThe resultant product was mixed with the filtrate
  10. washwashed with 50% methanol aqueous solution and saturated saline in this order
  11. dry with materialdried over anhydrous magnesium sulfate
  12. customThe solvent was evaporated

출처 및 근거

ORD 기록
ord-a6e1e44d925444beb2eaa4a288b12dc0
출처 데이터셋
uspto-grants-2011_08
특허 번호
US08003006B2

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