참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hexahydro-1,4-diazepine | HCID 68163 | — |
| 반응물 | Sodium Acetate | HCID 517045 | — |
| 반응물 | Ethyl 6-chloronicotinate | HCID 2799611 | — |
| 반응물 | Sodium Diacetate | HCID 23662384 | — |
| 반응물 | HCID 178506865 | HCID 178506865 | — |
| 용매 | Acetic Acid | HCID 176 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 1-[(6-Chloropyridin-3-yl)carbonyl]-1,4-diazepane | HCID 50999919 | — |
반응 단계
A solution of homopiperazine (385.62 g, 3.85 mol) in THF (3.9 L) was cooled to an internal temperature of 0° C. and ethyl 6-chloronicotinate (285.82 g, 1.54 mol) was added in THF (0.57 L) over 5 min. After stirring for 10 minutes, n-hexyl lithium (2.3 M in hexane, 335 mL, 0.77 mol) was added to the resulting mixture, over 40 min. The resulting mixture was stirred for 2 h at 0° C., then warmed to 20° C. over 1 h. After an additional 15 h at 20° C., the resulting mixture was treated with 1M NaOAc/HOAc buffer (5 L) (prepared by diluting 47.35 g of sodium acetate and 253.2 mL of acetic acid with water to a total volume of 5 L).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08748596B2 |
|---|
| 출처 데이터셋 | uspto-grants-2014_06 |
|---|
| ORD ID | ord-9aa9b603fd9940b2a0eba66ac817f0d4 |
|---|
| 출처 메모 | uspto-grants-2014_06 |
|---|
