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Hydrochloric Acid → Tert-butyl 3-(n-{(1r)-1-[(4-chlorophenyl)methyl]-2-oxo-2-[4-(2-pyridylmethyl)-piperazinyl]ethyl}carbamoyl)-(3s)-1,2,3,4-tetrahydroisoquinoline-2-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | HOAt | HCID 181649 | — |
| 反応物 | (3S)-2-((tert-butoxy)carbonyl)-1,2,3,4-tetrahydroisoquinoline-3-carboxylic acid | HCID 664088 | — |
| 反応物 | N-(3-dimethylaminopropyl)-N'-ethylcarbodiimide methyliodide | HCID 10236463 | — |
| 反応物 | n-{(1r)-1-[(4-Chlorophenyl)methyl]-2-oxo-2-[4-(2-pyridylmethyl)piperazinyl]ethyl}(tert-butoxy) carboxamide | HCID 69073501 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | Tert-butyl 3-(n-{(1r)-1-[(4-chlorophenyl)methyl]-2-oxo-2-[4-(2-pyridylmethyl)-piperazinyl]ethyl}carbamoyl)-(3s)-1,2,3,4-tetrahydroisoquinoline-2-carboxylate | HCID 69081076 | — |
反応手順
tert-Butyl 3-(N-{(1R)-1-[(4-chlorophenyl)methyl]-2-oxo-2-[4-(2-pyridylmethyl)-piperazinyl]ethyl}carbamoyl)-(3S)-1,2,3,4-tetrahydroisoquinoline-2-carboxylate was prepared from N-{(1R)-1-[(4-chlorophenyl)methyl]-2-oxo-2-[4-(2-pyridylmethyl)piperazinyl]ethyl}(tert-butoxy)carboxamide (Step 1) (270 mg, 0.58 mmol) according to the procedure used for Example 93, Step 2 using 25 mL HCl satd EtOAc, for the first step, then DIEA (100 μl, 0.574 mmol), Boc-L-Tic-OH (82 mg, 0.296 mmol), 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide methiodide (101 mg, 0.340 mmol), and HOAT (50 mg, 0.367 mmol) for the second step (139 mg). MS (ESI, pos. ion) m/z: 618 (M+H), (ESI, neg. ion) m/z: 616 (M−H). Calc'd for C34H40ClN5O4: 618.17.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07560460B2 |
| 出典データセット | uspto-grants-2009_07 |
| ORD ID | ord-688c32ad1763480198d8f16c8ed68729 |
| 出典メモ | uspto-grants-2009_07 |