Water → lanthanum (R)-1,1'-bi-2-naphthol

HRID 52610

반응식

HRID 52610 반응식
[Cl-].[Cl-].[Cl-].[La+3:4].[Li].C([Li])CCC.[CH:11]1[CH:16]=[C:15]2[CH:17]=[CH:18][C:19]([OH:32])=[C:20]([C:21]3[C:30]4[C:25](=[CH:26][CH:27]=[CH:28][CH:29]=4)[CH:24]=[CH:23][C:22]=3[OH:31])[C:14]2=[CH:13][CH:12]=1.CC(C)([O-])C.[Na+].O>C1COCC1.CCCCCC>[La:4].[CH:27]1[CH:26]=[C:25]2[CH:24]=[CH:23][C:22]([OH:31])=[C:21]([C:20]3[C:14]4[C:15](=[CH:16][CH:11]=[CH:12][CH:13]=4)[CH:17]=[CH:18][C:19]=3[OH:32])[C:30]2=[CH:29][CH:28]=1

참가 물질

9

반응물 6

HCID 962WaterHCID 11762BinolHCID 3028194LithiumHCID 9859665Lanthanum(III)chlorideHCID 23676156Sodium t-butoxideHCID 178418339Butyllithium

생성물 1

HCID 131719953lanthanum (R)-1,1'-bi-2-naphthol

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매3회HCID 8058Hexane용매

실험 절차

To a suspension of 122.6 mg (0.50 mmol) of anhydrous lanthanum trichloride in 6.0 ml of THF were added, in an argon atmosphere and at room temperature, a lithium binaphthoxide solution in THF [prepared by adding 0.625 ml (1.0 mmol) of a 1.6N n-butyllithium solution in hexane to a solution of 143.2 mg (0.50 mmol) of (R)-1,1'-bi-2-naphthol in 2.5 ml of THF], 48.1 mg (0.50 mmol) of sodium t-butoxide and 99 μl (5.5 mmol) of water in that order. The resultant mixture was stirred at room temperature for 15 hours. The insoluble matter was caused to precipitate by allowing the mixture to stand overnight, and the supernatant was submitted to the reaction proper as a lanthanum/(R)-1,1'-bi-2-naphthol complex solution (0.05 mol/l).

후처리

  1. additionwere added, in an argon atmosphere and at room temperature
  2. customto precipitate
  3. customthe supernatant was submitted to the reaction proper as a lanthanum/(R)-1,1'-bi-2-naphthol complex solution (0.05 mol/l)

출처 및 근거

ORD 기록
ord-c6ead5f7cab94cd1a2864511ea800122
출처 데이터셋
uspto-grants-1997_04
특허 번호
US05616726

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