Potassium Sodium Tartrate → 1,4-Butanediol, 2,2-diphenyl-

HRID 975111

반응식

HRID 975111 반응식
[C:1]1([C:7]2([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=3)[CH2:12][CH2:11][O:10][C:8]2=[O:9])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[H-].[Al+3].[Li+].[H-].[H-].[H-].[C@H](O)(C([O-])=O)[C@@H](O)C([O-])=O.[Na+].[K+]>C1COCC1>[C:1]1([C:7]([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)([CH2:12][CH2:11][OH:10])[CH2:8][OH:9])[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

참가 물질

5

반응물 3

HCID 9357Potassium Sodium TartrateHCID 70393Dihydro-3,3-diphenyl-2(3H)-furanoneHCID 21226445Aluminium lithium hydride

생성물 1

HCID 112419701,4-Butanediol, 2,2-diphenyl-수율 98.3%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

In anhydrous THF (80 ml) was dissolved α,α-diphenyl-γ-butyrolactone (7 g) followed by addition of lithium aluminum hydride (1 g) with ice-cooling, and the mixture was stirred under the same conditions for 3 hours. Then, under ice-cooling, a saturated aqueous solution of Rochelle salt was added dropwise to precipitate the aluminum and other inorganic matter. The supernatant was taken by decantation, dried and concentrated under reduced pressure. The residue was recrystallized from isopropyl ether to provide 2,2-diphenyl-1,4-butanediol (7 g).

후처리

  1. temperaturecooling
  2. temperatureThen, under ice-cooling
  3. customto precipitate the aluminum and other inorganic matter
  4. customdried
  5. concentrationconcentrated under reduced pressure
  6. customThe residue was recrystallized from isopropyl ether

출처 및 근거

ORD 기록
ord-45049620f24a441a9c4d9dd562ca185b
출처 데이터셋
uspto-grants-1997_03
특허 번호
US05607939

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