Sodium metaborate → HCID 54065558, 화합물

HRID 264912

반응식

HRID 264912 반응식
[CH2:1]([O:8][C:9]1[CH:16]=[CH:15][C:12]([CH:13]=[O:14])=[CH:11][C:10]=1[O:17][CH2:18][CH2:19][CH2:20][O:21][CH3:22])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.B([O-])=O.[Na+]>C(O)C.O>[CH2:1]([O:8][C:9]1[CH:16]=[CH:15][C:12]([CH2:13][OH:14])=[CH:11][C:10]=1[O:17][CH2:18][CH2:19][CH2:20][O:21][CH3:22])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

참가 물질

4

반응물 2

HCID 145326Sodium metaborateHCID 214586084-(Benzyloxy)-3-(3-methoxypropoxy)benzaldehyde

생성물 1

HCID 54065558HCID 54065558, 화합물

시약·촉매·용매 1

HCID 19096565Water ethanol용매2회

반응 조건

온도
0 °C

실험 절차

A solution of 31 g of 4-benzyloxy-3-(3-methoxypropyloxy)-benzaldehyde in 530 ml of ethanol/water=8:2 is added dropwise to a suspension, stirred at 0° C., of 11.74 g of sodium boranate in 530 ml of a mixture of ethanol/water=8:2. The reaction mixture is stirred for one hour at 0° C. and is then concentrated by evaporation. The residue is partitioned between diethyl ether and water. The combined organic phases are dried over sodium sulfate and concentrated by evaporation, and the residue is purified by FC (100 g of silica gel, dichloromethane/diethyl ether=1:1), yielding the title compound: Rf (dichloromethane/diethyl ether=1:1)=0.43.

후처리

  1. concentrationis then concentrated by evaporation
  2. customThe residue is partitioned between diethyl ether and water
  3. dry with materialThe combined organic phases are dried over sodium sulfate
  4. concentrationconcentrated by evaporation
  5. customthe residue is purified by FC (100 g of silica gel, dichloromethane/diethyl ether=1:1)

출처 및 근거

ORD 기록
ord-203cc9548934400e91597e87c78c9044
출처 데이터셋
uspto-grants-1997_07
특허 번호
US05646143

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