Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Dichloromethane → Ammonia dichloromethane
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Dichloromethane | HCID 6344 | — |
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 반응물 | 4-Phenylpiperidin-4-ol | HCID 96387 | — |
| 반응물 | 4-(3-Piperidin-1-ylpropoxy)benzaldehyde | HCID 2766324 | — |
| 반응물 | Sodium triacetoxyborohydride | HCID 5049666 | — |
| 용매 | Acetic Acid | HCID 176 | — |
| 생성물 | 4-Phenyl-1-[4-(3-piperidin-1-yl-propoxy)-benzyl]-piperidin-4-ol | HCID 10223185 | — |
| 생성물 | Ammonia dichloromethane | HCID 22731429 | 1% |
반응 단계
A solution of the product of Example 9 (210 mg), 4-Phenyl-piperidin-4-ol (150 mg), and acetic acid (0.05 mL) in DCM (3 mL) was treated with sodium triacetoxyborohydride (290 mg). After 16 h, the resulting mixture was treated with 10% sodium hydroxide (5 mL) and extracted with DCM (3×10 mL). The combined organic phases were dried (sodium sulfate) and evaporated. Chromatography of the residue (1-5% 2 M methanolic ammonia/DCM) gave the title compound as a colorless oil (225 mg). 1H NMR (400 MHz, CDCl3): 7.54-7.49 (m, 2H), 7.37-7.33 (m, 2H), 7.28-7.23 (m, 3H), 6.88-6.84 (m, 2H), 3.99 (t, J=6.3 Hz, 2H), 3.51 (s, 2H), 2.78 (m, 2H), 2.50-2.36 (m, 8H), 2.15 (m, 2H), 1.97 (m, 2H), 1.73 (m, 2H), 1.63-1.55 (m, 4H), 1.47-1.40 (m, 2H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07429586B2 |
| 출처 데이터셋 | uspto-grants-2008_09 |
| ORD ID | ord-dbdea33fac0c4bb78f92332e09f2f2db |
| 출처 메모 | uspto-grants-2008_09 |