Hydrochloric Acid → 2-(Tert-butylsulfamoyl)acetic acid

HRID 553465

反応式

HRID 553465 の反応式
C([O:3][C:4](=[O:14])[CH2:5][S:6](=[O:13])(=[O:12])[NH:7][C:8]([CH3:11])([CH3:10])[CH3:9])C.[OH-].[Na+].Cl>CCO.O>[C:8]([NH:7][S:6]([CH2:5][C:4]([OH:14])=[O:3])(=[O:13])=[O:12])([CH3:11])([CH3:9])[CH3:10]

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 19833529ethyl-2-(N-tert-butylsulfamoyl)acetate

生成物 1

HCID 287734162-(Tert-butylsulfamoyl)acetic acid収率 69%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

To a solution of ethyl-2-(N-tert-butylsulfamoyl)acetate (4 g, 17.9 mmol.) in 65 mL of EtOH and 13 mL of H2O at 0° C. was slowly added NaOH (3.6 g, 89.5 mmol.). The reaction was allowed to room temperature and stirred overnight. TLC analysis showed the reaction complete. The mixture was acidified to pH=5 with aq. HCl (1M). The resulting mixture was extracted with EtOAc (30 mL×3). The combined organic layer was dried over Na2SO4, concentrated to afford crude 2-(N-tert-butylsulfamoyl)acetic acid (2.4 g, 69%), which was used directly without purification.

後処理

  1. customat 0° C.
  2. customwas allowed to room temperature
  3. extractionThe resulting mixture was extracted with EtOAc (30 mL×3)
  4. dry with materialThe combined organic layer was dried over Na2SO4
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-2407a5ae7760488f90a884c11ea4060b
出典データセット
uspto-grants-2011_11
特許番号
US08048862B2

関連ノート

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