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

HRID 52611

반응식

HRID 52611 반응식
[CH:1]1[CH:6]=[C:5]2[CH:7]=[CH:8][C:9]([OH:22])=[C:10]([C:11]3[C:20]4[C:15](=[CH:16][CH:17]=[CH:18][CH:19]=4)[CH:14]=[CH:13][C:12]=3[OH:21])[C:4]2=[CH:3][CH:2]=1.C([Li])CCC.CC(C)[O-].[La+3:32].CC(C)[O-].CC(C)[O-]>C1COCC1.CCCCCC>[La:32].[CH:17]1[CH:16]=[C:15]2[CH:14]=[CH:13][C:12]([OH:21])=[C:11]([C:10]3[C:4]4[C:5](=[CH:6][CH:1]=[CH:2][CH:3]=4)[CH:7]=[CH:8][C:9]=3[OH:22])[C:20]2=[CH:19][CH:18]=1

참가 물질

6

반응물 3

HCID 11762BinolHCID 9858075Lanthanum isopropoxideHCID 178418339Butyllithium

생성물 1

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

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매HCID 8058Hexane용매

실험 절차

To a solution of 258 mg (0.90 mmol) of (R)-1,1'-bi-2-naphthol in 4.5 ml of THF Was added dropwise 0.56 ml (0.90 mmol) of a 1.6N n-butyllithium solution in hexane, at 0° C. in an argon atmosphere. After completion of the dropping, the temperature was raised to room temperature, 95 mg (0.30 mmol) of powdery lanthanum isopropoxide was added, and the mixture was stirred at room temperature for 15 hours. The insoluble matter was allowed to precipitate and the supernatant was submitted, as a lanthanum/(R)-1,1'-bi-2-naphthol complex solution (0.05 mol/l), to the reaction proper.

후처리

  1. customat 0° C.
  2. customto precipitate
  3. customthe supernatant was submitted, as a lanthanum/(R)-1,1'-bi-2-naphthol complex solution (0.05 mol/l), to the reaction proper

출처 및 근거

ORD 기록
ord-22026acd963c477fa474a5b7f1fb1c7d
출처 데이터셋
uspto-grants-1997_04
특허 번호
US05616726

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