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Potassium bisulfate → benzyl N-[3-(2-aminoethyl)pyrrolidine-1-carboximidoyl]carbamate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium bisulfate | HCID 516920 | — |
| 反応物 | tert-butyl N-[2-(pyrrolidin-3-yl)ethyl]carbamate | HCID 21955469 | — |
| 反応物 | Benzyl [amino(methylsulfanyl)methylene]carbamate | HCID 140362141 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | benzyl N-[3-(2-aminoethyl)pyrrolidine-1-carboximidoyl]carbamate | HCID 140379083 | 67.5% |
反応手順
2.18 g (0.0102 mole) (3RS)-3-(N-tert-butyloxycarbonylaminoethyl) pyrrolidine and 2.81 g (0.0125 mole) N-benzyloxycarbonyl-S-methylisothiourea was dissolved in 30 ml toluene and heated to 60°-70° C. for eight hours followed by stirring at room temperature for one day. 0.3M KHSO4 -solution was added and the water layer was washed with a mixture of the toluene and ethyl acetate and left for 2 days under which time the Boc group was removed. The acidic water phase was made alkaline and extracted four times with CH2 Cl2. The combined organic layer was dried (Na2SO4), filtered and evaporated to yield 2.0 g (51%) of the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05723444 |
| 出典データセット | uspto-grants-1998_03 |
| ORD ID | ord-d42f48a7d3fc473aba6c5139093935b5 |
| 出典メモ | uspto-grants-1998_03 |