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Trifluoroacetic acid → 2-Methyl-4-phenyl-2,8-diazaspiro[4.6]undecan-1-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Trifluoroacetic acid | HCID 6422 | — |
| 反応物 | Tert-butyl 2-methyl-1-oxo-4-phenyl-2,8-diazaspiro[4.6]undecane-8-carboxylate | HCID 71060314 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2-Methyl-4-phenyl-2,8-diazaspiro[4.6]undecan-1-one | HCID 71060546 | — |
反応手順
A diastereomeric mixture of tert-butyl 2-methyl-1-oxo-4-phenyl-2,8-diazaspiro[4.6]undecane-8-carboxylate (step 4) (683.1 mg; 1.906 mmol) in DCM (6 ml) was treated with TFA (5.8 ml, 76 mmol) and stirred at RT for 10 minutes. The mixture was concentrated in vacuo and the crude product was dissolved in MeOH and applied to a 10 g pre-wetted (MeOH) SCX-2 cartridge. The column was washed with MeOH and the product was eluted with 2M NH3 in MeOH. The clean fractions were concentrated in vacuo to afford the title compound;
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08546416B2 |
| 出典データセット | uspto-grants-2013_10 |
| ORD ID | ord-db267e25f8a342568ff8cd2bdc581362 |
| 出典メモ | uspto-grants-2013_10 |