関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Chloroethane | HCID 6337 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Benzyl chloroformate | HCID 10387 | — |
| 反応物 | 4-Acetamido-4-phenyl-1-[2-[1-(3,4-dichlorophenyl)-2-(N-methylamino)ethoxy]ethyl]piperidine dihydrochloride | HCID 19692500 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4-Acetamido-4-phenyl-1-[2-[1-(3,4-dichlorophenyl)-2-(N-methyl-N-benzyloxycarbonylamino)ethoxy]ethyl]piperidine hydrochloride | HCID 19692462 | — |
反応手順
0.41 ml of triethylamine is added to a solution of 0.5 g of the compound obtained in EXAMPLE 11, step B), in 10 ml of DCM, the mixture is then cooled to 0° C. and 0.14 ml of benzyl chloroformate is added dropwise. The reaction mixture is washed twice with water, dried over MgSO4 and concentrated under vacuum. The residue is chromatographed on silica gel H using DCM and then a DCM/MeOH mixture (94/6; v/v) as the eluent. The product obtained is taken up with DCM, acidified to pH 1 by the addition of hydrochloric ether and concentrated under vacuum to give 0.39 g of the expected hydrochloride after crystallization from iso ether. M.p.=135° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05726313 |
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| 出典データセット | uspto-grants-1998_03 |
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| ORD ID | ord-7d504e6d31bb4728a49a96e042f2ee0f |
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| 出典メモ | uspto-grants-1998_03 |
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