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Triphosgene → 3-[(S)-1-(3,4-Difluoro-phenyl)-ethyl]-1-oxa-3-aza-spiro[5.5]undecane-2,9-dione
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triphosgene | HCID 94429 | — |
| 反応物 | 3-[(S)-1-(3,4-difluoro-phenyl)-ethyl]-12,12-dimethyl-1,10,14-trioxa-3-aza-dispiro[5.2.5.2]hexadecan-2-one | HCID 67995860 | — |
| 反応物 | 9-{2-[(S)-1-(3,4-Difluoro-phenyl)-ethylamino]-ethyl}-3,3-dimethyl-1,5-dioxa-spiro[5.5]undecan-9-ol | HCID 67996346 | — |
| 生成物 | 3-[(S)-1-(3,4-Difluoro-phenyl)-ethyl]-1-oxa-3-aza-spiro[5.5]undecane-2,9-dione | HCID 56595758 | — |
反応手順
The title compound is prepared from 9-{2-[(S)-1-(3,4-difluoro-phenyl)-ethylamino]-ethyl}-3,3-dimethyl-1,5-dioxa-spiro[5.5]undecan-9-ol and triphosgene following a procedure analogous to that described in Step 4 of Intermediate 2; the crude product, a mixture of the title compound and 3-[(S)-1-(3,4-difluoro-phenyl)-ethyl]-12,12-dimethyl-1,10,14-trioxa-3-aza-dispiro[5.2.5.2]hexadecan-2-one, obtained after that is treated as described in Step 10 of Intermediate 2 to convert the intermediate to the title compound, too. Yield: 68% of theory; LC (method 6): tR=1.14 min; Mass spectrum (ESI+): m/z=324 [M+H]+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08765744B2 |
| 出典データセット | uspto-grants-2014_07 |
| ORD ID | ord-1a618c5d1cf145bbb72c6b7be664f819 |
| 出典メモ | uspto-grants-2014_07 |