Hydrochloric Acid → HCID 58415292、化合物

HRID 2075243ノート

反応式

HRID 2075243 の反応式
[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

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 1061PhosphateHCID 3939Lithium HydroxideHCID 58415364HCID 58415364、化合物

生成物 1

HCID 58415292HCID 58415292、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-60f071d68d6447558a8aa14dd20d378c
出典データセット
uspto-grants-2011_04
特許番号
US07919519B2

反応ノート

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