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Hydrogen Sulfide → 2-Amino-2-benzyloxymethyl-1-phthalimido-ethane
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrogen Sulfide | HCID 402 | — |
| 反応物 | 2-Benzyloxymethyl-2-azido-1-phthalimido-ethane | HCID 19438532 | — |
| 反応物 | Pyridine water | HCID 66926435 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 2-Amino-2-benzyloxymethyl-1-phthalimido-ethane | HCID 19438552 | 20% |
反応手順
Into a stirred solution of 2-benzyloxymethyl-2-azido-1-phthalimido-ethane (500 mg, 1.5 mmol) in 4:1 pyridine/water (25 ml) was bubbled hydrogen sulphide, and the reaction was monitored by TLC. After 4 hours, the gas flow was stopped, and the reaction flask sealed. The intense green reaction mixture was stirred for another 17 hours. TLC indicated full conversion of the starting material. Glacial acetic acid was added to pH 7, and the reaction mixture was evaporated to dryness in vacuo. After evaporation from ethanol (3×25 ml), the resulting brown solid was purified by chromatography. Yield=20%. The structure was confirmed by NMR and IR.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05198208 |
| 出典データセット | uspto-grants-1993_03 |
| ORD ID | ord-54a2dcf0bd174ba5a3ad293f2af038dd |
| 出典メモ | uspto-grants-1993_03 |