Hydrochloric Acid → 1-[3-[5-[(2(S)-Azetidinyl)methoxy]-3-pyridyl]phenyl]-3-phenyl-2(R)-propanol Hydrochloride

HRID 2095351노트

반응식

HRID 2095351 반응식
[NH:1]1[CH2:4][CH2:3][C@H:2]1[CH2:5][O:6][C:7]1[CH:8]=[C:9]([C:13]2[CH:14]=[C:15]([CH2:19][C@H:20]([OH:28])[CH2:21][C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=3)[CH:16]=[CH:17][CH:18]=2)[CH:10]=[N:11][CH:12]=1.[ClH:29]>CO>[ClH:29].[NH:1]1[CH2:4][CH2:3][C@H:2]1[CH2:5][O:6][C:7]1[CH:8]=[C:9]([C:13]2[CH:14]=[C:15]([CH2:19][C@H:20]([OH:28])[CH2:21][C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=3)[CH:16]=[CH:17][CH:18]=2)[CH:10]=[N:11][CH:12]=1

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 461913501-[3-[5-[(2(S)-azetidinyl)methoxy]-3-pyridyl]phenyl]-3-phenyl-2(R)-propanol

생성물 1

HCID 686116921-[3-[5-[(2(S)-Azetidinyl)methoxy]-3-pyridyl]phenyl]-3-phenyl-2(R)-propanol Hydrochloride

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a solution of 1-[3-[5-[(2(S)-azetidinyl)methoxy]-3-pyridyl]phenyl]-3-phenyl-2(R)-propanol (130 mg, 0.35 mmol) in methanol (1 mL) was added 2M hydrochloric acid (0.4 mL) at 0° C. under N2. The solution was stirred for 2 h at room temperature and then evaporated. Water (8 mL) was added to dissolve the residue, and the solution was lyophilized. The residue was dissolved in 12 mL of water, and the solution was re-lyophilized to give the hydrochloride (145 mg) as a colorless solid. 1H NMR (D2O, 300 MHz) δ 8.65 (s, 1H), 8.51 (s, 1H), 8.38 (s, 1H), 7.58-7.47 (m, 3H), 7.42-7.39 (m, 1H), 7.32-7.22 (m, 5H), 4.99-4.94 (m, 1H), 4.57 (d, 2H, J=3.9 Hz), 4.17-4.03 (m, 3H), 2.99-2.63 (m, 6H). Anal. Calcd. for C24H26N2O2.2.45HCl.1.65H2O: C, 58.41; H, 6.48; N, 5.68; Cl, 17.60. Found: C, 58.51; H, 6.69; N, 5.58; Cl, 17.66.

후처리

  1. customevaporated
  2. additionWater (8 mL) was added
  3. dissolutionto dissolve the residue
  4. dissolutionThe residue was dissolved in 12 mL of water

출처 및 근거

ORD 기록
ord-2e0ae21241884541b7ef7f57e3fef291
출처 데이터셋
uspto-grants-2013_05
특허 번호
US08445684B2

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