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HRID 2944作成日:2026年10月24日

Ammonium Hydroxide → 5-[[3,5-Bis(1,1-dimethylethyl)-4-hydroxyphenyl]methylene]-3-(2-hydroxyethyl)-4-thiazolidinone

https://huagongshe.com/ja/reaction/2944

反応式

関与物質

役割名称HCID仕込み量
反応物Ammonium HydroxideHCID 14923—
反応物5-[[3,5-Bis(1,1-dimethylethyl)-4-hydroxyphenyl]methylene]-3-[2-(acetyloxy)ethyl]-4-thiazolidinoneHCID 53867199—
溶媒AcetonitrileHCID 6342—
生成物5-[[3,5-Bis(1,1-dimethylethyl)-4-hydroxyphenyl]methylene]-3-(2-hydroxyethyl)-4-thiazolidinoneHCID 5450750246.7%

反応手順

A solution of 85.2 g of 5-[[3,5-bis(1,1-dimethylethyl) -4-hydroxyphenyl]methylene]-3-[2-(acetyloxy)ethyl]-4-thiazolidinone from Example 26 in 1.5 l of acetonitrile was treated with 1 liter of concentrated ammonium hydroxide. The reaction mixture was allowed to stand for approximately 90 hours at room temperature. The solution was concentrated in vacuo and 500 ml of ethyl acetate were added, with the pH adjusted to 3.0 with concentrated hydrochloric acid. The layers were separated and the aqueous layer extracted with 250 ml of ethyl acetate. The combined organic layers were washed with 250 ml of a saturated sodium chloride solution and concentrated in vacuo. The residue was crystallized from 95 ml of hexane and 70 ml of ethyl acetate to provide 35.68 g of the desired subtitled intermediate, m.p. 131°-135° C.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US05731336
出典データセットuspto-grants-1998_03
ORD IDord-dab83e5f8e4f453e9acc6425fd301ce5
出典メモuspto-grants-1998_03