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HRID 1696695作成日:2026年10月27日

Dichloromethane → 2-[(2-Hydroxy-1-methyl-2-{4-[(triisopropylsilyl)oxy]phenyl}ethyl)thio]phenol

https://huagongshe.com/reaction/1696695

反応式

関与物質

役割名称HCID仕込み量
反応物DichloromethaneHCID 6344—
反応物Ammonium ChlorideHCID 25517—
反応物Sodium borohydrideHCID 4311764—
反応物2-[(2-Hydroxyphenyl)thio]-1-{4-[(triisopropylsilyl)oxy]phenyl}propan-1-oneHCID 67277409—
溶媒MethanolHCID 887—
生成物2-[(2-Hydroxy-1-methyl-2-{4-[(triisopropylsilyl)oxy]phenyl}ethyl)thio]phenolHCID 67277626106.1%

反応手順

With cooling with ice, sodium borohydride (5.5 g, 134 mmol) was added to a dichloromethane (500 mL)/methanol (500 mL) mixed solution of 2-[(2-hydroxyphenyl)thio]-1-{4-[(triisopropylsilyl)oxy]phenyl}propan-1-one (48 g, 112 mmol) obtained in Reference Example 1-2, and stirred for 2 hours with cooling with ice, then restored to room temperature, and further stirred for 40 minutes. Aqueous saturated ammonium chloride solution was added, and stirred for a while, and then the solvent was almost completely evaporated off under reduced pressure. The residue was diluted with ethyl acetate, and extracted with aqueous saturated ammonium chloride solution. The organic layer was dried with sodium sulfate, and concentrated under reduced pressure to obtain a crude product (51.4 g) of the intended compound.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US08163770B2
出典データセットuspto-grants-2012_04
ORD IDord-31c3d690cf844e988d754e0954d94b54
出典メモuspto-grants-2012_04