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Lithium Hydroxide → (3R)-4-(4-toluenesulfonyl)thiomorpholine-3-carboxylic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Lithium Hydroxide | HCID 3939 | — |
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | (3R)-4-(4-toluenesulfonyl)thiomorpholine-3-carboxylic acid methyl ester | HCID 69416803 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | (3R)-4-(4-toluenesulfonyl)thiomorpholine-3-carboxylic acid | HCID 69415969 | 97.1% |
反応手順
8.3 g of (3R)-4-(4-toluenesulfonyl)thiomorpholine-3-carboxylic acid methyl ester was dissolved in 157 mL of methanol and 52.5 ml 1 mol/L of LiOH solution was added dropwise in the above solution at 0° C. The mixture was stirred for 48 h and ethyl acetate (60, 60 ml) was added into the reaction mixture and separated to collect mother liquid. The mother liquid was acidified by 100 ml 1 mol/L hydrogen chloride to adjust pH value to 2. Filtrated and collected the white solid to obtain 7.7 g product. Yield 97.0%□mp149-150° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07304057B2 |
| 出典データセット | uspto-grants-2007_12 |
| ORD ID | ord-df3cdd5c4a114f0b8cca63a0c2f282a8 |
| 出典メモ | uspto-grants-2007_12 |