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Hydrochloric Acid → HCID 59253266、化合物

HRID 643695
ノート
印刷プレビュー

反応式

HRID 643695 の反応式
[CH:1]1([CH2:4][N:5]2[C:9]3[CH:10]=[CH:11][C:12]([S:14]([C:17]([CH3:23])([CH3:22])[C:18]([O:20]C)=[O:19])(=[O:16])=[O:15])=[CH:13][C:8]=3[N:7]=[C:6]2[CH2:24][C:25]([CH3:28])([CH3:27])[CH3:26])[CH2:3][CH2:2]1.[OH-].[Na+].Cl>CO.O1CCCC1>[CH:1]1([CH2:4][N:5]2[C:9]3[CH:10]=[CH:11][C:12]([S:14]([C:17]([CH3:22])([CH3:23])[C:18]([OH:20])=[O:19])(=[O:16])=[O:15])=[CH:13][C:8]=3[N:7]=[C:6]2[CH2:24][C:25]([CH3:28])([CH3:27])[CH3:26])[CH2:2][CH2:3]1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 59253268HCID 59253268、化合物

生成物 1

HCID 59253266HCID 59253266、化合物収率 89%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of methyl 2-{[1-(cyclopropylmethyl)-2-(2,2-dimethylpropyl)-1H-benzimidazol-5-yl]sulfonyl}-2-methylpropanoate (Step G, 1.07 g, 2.64 mmol) in methanol (5 mL) and tetrahydrofuran (5 mL) was added 2N sodium hydroxide aqueous solution (5 mL) at room temperature. The mixture was stirred at room temperature for 3 h. The mixture was made acidic with 2N hydrochloric acid (pH ˜4) and concentrated under reduced pressure. The residue was dissolved in water (50 mL) and dichloromethane (50 mL). The aqueous layer was separated and extracted with dichloromethane (50 mL×2). The combined organic layers were dried over magnesium sulfate and concentrated under reduced pressure to afford the title compound (920 mg, 89%) as a white solid.

後処理

  1. concentrationconcentrated under reduced pressure
  2. dissolutionThe residue was dissolved in water (50 mL)
  3. customThe aqueous layer was separated
  4. extractionextracted with dichloromethane (50 mL×2)
  5. dry with materialThe combined organic layers were dried over magnesium sulfate
  6. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-865b343fb78842be8fdd81404c4c7127
出典データセット
uspto-grants-2010_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07700618B2

反応ノート

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