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

HRID 2095347ノート

反応式

HRID 2095347 の反応式
[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

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 593713341-[3-[5-[(2(S)-azetidinyl)methoxy]-3-pyridyl]phenyl]-3-phenyl-2(S)-propanol

生成物 1

HCID 686120371-[3-[5-[(2(S)-Azetidinyl)methoxy]-3-pyridyl]phenyl]-3-phenyl-2(S)-propanol Hydrochloride

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a solution of 1-[3-[5-[(2(S)-azetidinyl)methoxy]-3-pyridyl]phenyl]-3-phenyl-2(S)-propanol (130 mg, 0.35 mmol) in methanol (1 mL) was added 2M hydrochloric acid (0.53 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 (br s, 1H), 8.49 (br s, 1H), 8.35 (br s, 1H), 7.57-7.46 (m, 3H), 7.42 (m, 1H), 7.33-7.22 (m, 5H), 4.96 (m, 1H), 4.57 (d, 2H, J=3.9 Hz), 4.17-4.03 (m, 3H), 2.99-2.62 (m, 6H). LC-MS (ESI) m/z 375 (M+H+). Anal. Calcd. for C24H26N2O2.2.1HCl.1.25H2O: C, 60.87; H, 6.51; N, 5.92; Cl, 15.72. Found: C, 60.87; H, 6.50; N, 5.85; Cl, 15.61.

後処理

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

出典と根拠

ORDレコード
ord-63ebfac4fcec4c69a713313b02b70e97
出典データセット
uspto-grants-2013_05
特許番号
US08445684B2

反応ノート

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