Sodium metaborate → HCID 54065558、化合物

HRID 264912

反応式

HRID 264912 の反応式
[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

参加物

4

反応物 2

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

生成物 1

HCID 54065558HCID 54065558、化合物

試薬・触媒・溶媒 1

HCID 19096565Water ethanol溶媒2 回

反応条件

温度
0 °C

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-203cc9548934400e91597e87c78c9044
出典データセット
uspto-grants-1997_07
特許番号
US05646143

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