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Norcamphor → 1'-(bicyclo[2.2.1]heptan-2-yl)-N-methylspiro[indene-1,4'-piperidine]-3-carboxamide

HRID 2267112
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HRID 2267112 반응식
[CH3:1][NH:2][C:3]([C:5]1[C:18]2[C:13](=[CH:14][CH:15]=[CH:16][CH:17]=2)[C:7]2([CH2:12][CH2:11][NH:10][CH2:9][CH2:8]2)[CH:6]=1)=[O:4].[C@H:19]12[CH2:25][C@H:22]([CH2:23][CH2:24]1)[CH2:21][C:20]2=O.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+]>ClC(Cl)C.CC(C)[O-].[Ti+4].CC(C)[O-].CC(C)[O-].CC(C)[O-]>[CH:19]12[CH2:25][CH:22]([CH2:23][CH2:24]1)[CH2:21][CH:20]2[N:10]1[CH2:11][CH2:12][C:7]2([C:13]3[C:18](=[CH:17][CH:16]=[CH:15][CH:14]=3)[C:5]([C:3]([NH:2][CH3:1])=[O:4])=[CH:6]2)[CH2:8][CH2:9]1
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참가 물질

6

반응물 3

HCID 449588NorcamphorHCID 5049666Sodium triacetoxyborohydrideHCID 59600609N-methylspiro[indene-1,4'-piperidine]-3-carboxamide

생성물 1

HCID 596006101'-(bicyclo[2.2.1]heptan-2-yl)-N-methylspiro[indene-1,4'-piperidine]-3-carboxamide

시약·촉매·용매 2

HCID 11026Titanium isopropoxide촉매
HCID 6365
1,1-Dichloroethane
용매

실험 절차

A mixture of (C6) (0.015 g, 0.073 mmol), titanium (IV) isopropoxide (0.065 mL, 0.22 mmol) and (1R,4S)-bicyclo[2.2.1]heptan-2-one (3 eq) was stirred at room temperature for 18 h in dichloroethane (0.5 mL). Sodium triacetoxyborohydride (0.013 g, 0.073 mmol) was added and the reaction stirred at room temperature for 1 h. The solvent was evaporated and 6N NaOH (0.5 mL) and methanol (1 mL) was added and triturated to give a white solid. The solid was washed with methanol (1 mL) and EtOAc (1 mL). The filtrate was concentrated under reduced pressure to afford the crude product that was purified by reverse phase preparative HPLC to afford 1′-(bicyclo[2.2.1]heptan-2-yl)-N-methylspiro[indene-1,4′-piperidine]-3-carboxamide (Compound No. 38) (0.012 g) as an oil. LC/MS (10-90% over 3 min with 0.9% FA) m/z 337.2 (M+1), Rt 1.7 minutes. 1HNMR (500 MHz, CD3OD): δ 7.74 (d, 1H), 7.35 (m, 4H), 3.73 (m, 2H), 3.55 (m, 1H), 3.30 (m, 2H), 2.91 (s, 3H), 2.42-2.74 (m, 5H), 2.19 (m, 2H), 1.54-1.74 (m, 8H), 1.31 (m, 1H)

후처리

  1. customThe solvent was evaporated
  2. addition6N NaOH (0.5 mL) and methanol (1 mL) was added
  3. customtriturated
  4. customto give a white solid
  5. washThe solid was washed with methanol (1 mL) and EtOAc (1 mL)
  6. concentrationThe filtrate was concentrated under reduced pressure
  7. customto afford the crude product that
  8. customwas purified by reverse phase preparative HPLC

출처 및 근거

ORD 기록
ord-1671c58fd0e844ef8089ea1db088bef2
출처 데이터셋
uspto-grants-2010_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07858790B2

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