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Sodium Methoxide → 4-(3-Methylbutyl)-5-methyl-1,2,5-thiadiazolidin-3-one 1,1-dioxide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Methoxide | HCID 10942334 | — |
| 反応物 | N-(aminosulfonyl)-2-(3-methylbutyl)sarcosine methyl ester | HCID 18922252 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 4-(3-Methylbutyl)-5-methyl-1,2,5-thiadiazolidin-3-one 1,1-dioxide | HCID 18922262 | 99.8% |
反応手順
A solution of N-(aminosulfonyl)-2-(3-methylbutyl)-sarcosine methyl ester (12.28 g, 48.67 mmol) in methanol (150 ml) was added under nitrogen to a solution of sodium methoxide (Na=2.1 g, 95.71 mmol) ) in 150 ml of ice-cold methanol. The resulting reaction mixture was stirred at room temperature under nitrogen for 1.5 hours, and the mixture was treated with 25 g of ion-exchange resin (BIO-RAD 50W-x8 H+) for 40 minutes, and filtered. The filtrate was concentrated in vacuo to afford 10.7 g (99.8%) of 4-(3-methylbutyl)-5-methyl-1,2,5-thiadiazolidin-3-one 1,1-dioxide (Formula IV: R1 =H; R2= (CH2)2CH (CH3)2 ; R3 =CH3) as a solid, m.p. 212°-214° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05556909 |
| 出典データセット | uspto-grants-1996_09 |
| ORD ID | ord-dc59298c7b914b43bdfec91b982c82c3 |
| 出典メモ | uspto-grants-1996_09 |