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Sodium Hydroxide → HCID 44548889、化合物

HRID 1512920
ノート
印刷プレビュー

反応式

HRID 1512920 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([C:12]2[O:16][N:15]=[C:14]([C:17]3[CH:18]=[CH:19][CH:20]=[C:21]4[C:25]=3[NH:24][CH:23]=[C:22]4[CH2:26][CH2:27][NH:28][CH2:29][CH2:30][C:31]([O:33]CC)=[O:32])[N:13]=2)[CH:5]=[CH:6][C:7]=1[O:8][CH:9]([CH3:11])[CH3:10].[OH-].[Na+]>O1CCCC1.CO.O>[Cl:1][C:2]1[CH:3]=[C:4]([C:12]2[O:16][N:15]=[C:14]([C:17]3[CH:18]=[CH:19][CH:20]=[C:21]4[C:25]=3[NH:24][CH:23]=[C:22]4[CH2:26][CH2:27][NH:28][CH2:29][CH2:30][C:31]([OH:33])=[O:32])[N:13]=2)[CH:5]=[CH:6][C:7]=1[O:8][CH:9]([CH3:10])[CH3:11]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 2

HCID 14798Sodium HydroxideHCID 59146183HCID 59146183、化合物

生成物 1

HCID 44548889HCID 44548889、化合物収率 74.1%

試薬・触媒・溶媒 3

HCID 887Methanol溶媒HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

反応条件

温度
20 °C

実験手順

To a solution of ethyl N-{2-[7-(5-{3-chloro-4-[(1-methylethyl)oxy]phenyl}-1,2,4-oxadiazol-3-yl)-1H-indol-3-yl]ethyl}-β-alaninate (D85) (186 mg) in tetrahydrofuran (5 mL) and methanol (5 mL) stirred at 20° C. was added a solution of sodium hydroxide (40 mg) in water (5 mL) in one charge. The reaction mixture was stirred at 20° C. overnight. The reaction mixture was concentrated to about 5 mL and then HCl aquous solution was added dropwise until no further white precipitate was formed. The solid was filtered and washed with EtOAc. The solid was collected and then was suspended in methanol (5 mL) and water (5 mL). The mixture was acidified with HCl aquous solution to pH around 1 to form a clear solution. After most of the solvent was evaporated off, the residue was freeze-dried to afford N-{2-[7-(5-{3-chloro-4-[(1-methylethyl)oxy]phenyl}-1,2,4-oxadiazol-3-yl)-1H-indol-3-yl]ethyl}-β-alanine (E62) (130 mg) as a hydrochloride salt. δH (DMSO-d6, 400 MHz): 1.38 (6H, d), 2.70 (2H, t), 3.12-3.29 (4H, m), 3.33 (2H, m), 4.88-4.94 (1H, m), 7.27 (1H, t), 7.41 (1H, d), 7.47 (1H, d), 7.90 (1H, d), 7.99 (1H, dd), 8.22 (1H, dd), 8.39 (1H, d), 8.71 (1H, br), 11.03 (1H, br s), 12.70 (1H, br s). MS (ES): C24H26ClN4O4 requires 468; found 469.2 (M+H+).

後処理

  1. additioncharge
  2. concentrationThe reaction mixture was concentrated to about 5 mL
  3. additionHCl aquous solution was added dropwise until no further white precipitate
  4. customwas formed
  5. filtrationThe solid was filtered
  6. washwashed with EtOAc
  7. customThe solid was collected
  8. customto form a clear solution
  9. customAfter most of the solvent was evaporated off
  10. customthe residue was freeze-dried

出典と根拠

ORDレコード
ord-5b2c55475fe148ac836019d56bb78ebe
出典データセット
uspto-grants-2012_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08217028B2

反応ノート

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