Hydrochloric Acid → HCID 58415292, 화합물

HRID 2075243노트

반응식

HRID 2075243 반응식
[Li+].[OH-].[CH2:3]([C:10]1[CH:11]=[C:12]2[O:19][C:18]([C:20]3[CH:25]=[CH:24][C:23]([CH2:26][N:27]4[CH2:30][CH:29]([C:31]([O:33]C)=[O:32])[CH2:28]4)=[CH:22][C:21]=3[F:35])=[CH:17][C:13]2=[N:14][C:15]=1[Cl:16])[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1.P([O-])([O-])([O-])=O.Cl>O.C1COCC1>[CH2:3]([C:10]1[CH:11]=[C:12]2[O:19][C:18]([C:20]3[CH:25]=[CH:24][C:23]([CH2:26][N:27]4[CH2:30][CH:29]([C:31]([OH:33])=[O:32])[CH2:28]4)=[CH:22][C:21]=3[F:35])=[CH:17][C:13]2=[N:14][C:15]=1[Cl:16])[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 1061PhosphateHCID 3939Lithium HydroxideHCID 58415364HCID 58415364, 화합물

생성물 1

HCID 58415292HCID 58415292, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of LiOH (0.022 g, 0.90 mmol) in water (3.0 mL) was added methyl 1-((4-(6-benzyl-5-chlorofuro[3,2-b]pyridin-2-yl)-3-fluorophenyl)methyl)azetidine-3-carboxylate (0.084 g, 0.18 mmol) in THF (2.0 mL). The solution was stirred for 30 min and then the solvent was removed under reduced pressure to afford a white suspension. To the mixture was added 0.5M phosphate buffer, pH 6.0 (3 mL), and then 1 N HCl was added until the pH was 6.0 as indicated by pH paper. The resulting suspension was filtered, and the off white solid was collected and dried under vacuum at 50° C. 1H NMR (400 MHz, DMSO-d6 with 1 drop of TFA-d) 8 ppm 8.04-8.21 (2H, m), 7.44-7.70 (3H, m), 7.18-7.40 (5H, m), 4.45-4.60 (2H, m), 4.13-4.40 (6H, m), 3.60-3.76 (1H, m); MS (ESI) m/z: Calculated: 450.1; Observed: 451.1 (M++1).

후처리

  1. customthe solvent was removed under reduced pressure
  2. customto afford a white suspension
  3. filtrationThe resulting suspension was filtered
  4. customthe off white solid was collected
  5. customdried under vacuum at 50° C

출처 및 근거

ORD 기록
ord-60f071d68d6447558a8aa14dd20d378c
출처 데이터셋
uspto-grants-2011_04
특허 번호
US07919519B2

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