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Ammonia → 2-Amino-2-oxoethyl 4-[(1-naphthalenyl-oxy)methyl]-1-piperidinecarboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ammonia | HCID 222 | — |
| 反応物 | 2-(Ethyloxy)-2-oxoethyl 4-[(1-naphthalenyloxy)methyl]-1-piperidinecarboxylate | HCID 67416005 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 2-Amino-2-oxoethyl 4-[(1-naphthalenyl-oxy)methyl]-1-piperidinecarboxylate | HCID 11313868 | 83.6% |
反応手順
1.0 g (2.69 mmol) of 2-(ethyloxy)-2-oxoethyl 4-[(1-naphthalenyloxy)methyl]-1-piperidinecarboxylate, prepared in Step 7.3., is dissolved in 12 ml of a 7N solution of ammonia (84 mmol) in methanol. The solution is left to react at ambient temperature for 3 days. It is evaporated to dryness and the residue is purified by chromatography on silica gel, eluting with a 90/10 then 80/20, 70/30 and 50/50 mixture of dichloromethane and ethyl acetate and then with a 95/5 mixture of ethyl acetate and methanol. The eluate is subsequently recrystallized from ethyl acetate, to give 0.77 g of product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08026258B2 |
| 出典データセット | uspto-grants-2011_09 |
| ORD ID | ord-7cb3b477f3c44c33a0a7757a87263794 |
| 出典メモ | uspto-grants-2011_09 |