Hydrochloric Acid → 3-Benzyloxy-4-(1-tert-butoxycarbonylmethyl-2,2-diethyoxy-ethylsulfamoyl-)benzoic acid

HRID 1814358ノート

反応式

HRID 1814358 の反応式
C[O:2][C:3](=[O:38])[C:4]1[CH:9]=[CH:8][C:7]([S:10](=[O:29])(=[O:28])[NH:11][CH:12]([CH2:20][C:21]([O:23][C:24]([CH3:27])([CH3:26])[CH3:25])=[O:22])[CH:13]([O:17][CH2:18][CH3:19])[O:14][CH2:15][CH3:16])=[C:6]([O:30][CH2:31][C:32]2[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=2)[CH:5]=1.[OH-].[Li+].Cl>C(OCC)(=O)C>[CH2:31]([O:30][C:6]1[CH:5]=[C:4]([CH:9]=[CH:8][C:7]=1[S:10](=[O:28])(=[O:29])[NH:11][CH:12]([CH2:20][C:21]([O:23][C:24]([CH3:27])([CH3:26])[CH3:25])=[O:22])[CH:13]([O:17][CH2:18][CH3:19])[O:14][CH2:15][CH3:16])[C:3]([OH:38])=[O:2])[C:32]1[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 3939Lithium HydroxideHCID 697315433-Benzyloxy-4-(1-tert-butoxycarbonylmethyl-2,2-diethoxy-ethylsulfamoyl)-benzoic acid methyl ester

生成物 1

HCID 1317248233-Benzyloxy-4-(1-tert-butoxycarbonylmethyl-2,2-diethyoxy-ethylsulfamoyl-)benzoic acid収率 65%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

3-Benzyloxy-4-(1-tert-butoxycarbonylmethyl-2,2-diethoxy-ethylsulfamoyl)-benzoic acid methyl ester (6.82 g, 12.4 mmol) was combined and stirred with 1M lithium hydroxide (26 mL, 26 mmol) in tetrohydrofuran (250 mL) at room temperature overnight. The reaction mixture was diluted with ethyl acetate and acidified with 1M HCl (26 mL). The organic layer was collected and extracted with water, brine, dried over magnesium sulfate, filtered, and concentrated under reduced pressure to give 3-benzyloxy-4-(1-tert-butoxycarbonylmethyl-2,2-diethyoxy-ethylsulfamoyl-)benzoic acid (4.32 g, 8.0 mmol, 65%). MS (APCI) m/z 536.3 (M−1).

後処理

  1. customThe organic layer was collected
  2. extractionextracted with water, brine
  3. dry with materialdried over magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-b2824492aa2a4b70be01d1cda49bc815
出典データセット
uspto-grants-2005_04
特許番号
US06875765B2

反応ノート

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