Hydrochloric Acid → 4-Trifluoromethanesulfonylamino-butyryl chloride

HRID 723179ノート

反応式

HRID 723179 の反応式
C[O:2][C:3](=O)[CH2:4][CH2:5][CH2:6][NH:7][S:8]([C:11]([F:14])([F:13])[F:12])(=[O:10])=[O:9].[OH-].[Na+].Cl.S(Cl)([Cl:21])=O>CO.ClCCl.CN(C=O)C>[F:12][C:11]([F:14])([F:13])[S:8]([NH:7][CH2:6][CH2:5][CH2:4][C:3]([Cl:21])=[O:2])(=[O:10])=[O:9]

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 24386Thionyl ChlorideHCID 866011824-Trifluoromethanesulfonylamino-butyric acid methyl ester

生成物 1

HCID 218861334-Trifluoromethanesulfonylamino-butyryl chloride

試薬・触媒・溶媒 2

HCID 22350042dichloromethane N,N-dimethylformamide触媒HCID 887Methanol溶媒

実験手順

4-Trifluoromethanesulfonylamino-butyric acid methyl ester (0.42 g, 1.77 mmol) [example 212, step a] was taken up in methanol [2 mL] and 1N NaOH was added [2.66 mL] and stirred for 2 hours. 1N HCl was added and the product was extracted with ethyl acetate, dried with magnesium sulfate and evaporated. The crude product (0.13 g, 0.57 mmol) was dissolved in dichloromethane/DMF [1 mL/1 drop] and thionyl chloride (0.08 mL, 1.14 was added. The reaction was stirred at room temperature for 2 hours and then evaporated and used directly in the next step.

後処理

  1. extractionthe product was extracted with ethyl acetate
  2. dry with materialdried with magnesium sulfate
  3. customevaporated
  4. stirringThe reaction was stirred at room temperature for 2 hours
  5. customevaporated

出典と根拠

ORDレコード
ord-f2eaef2f06b8454f8c501cc0c102a7c6
出典データセット
uspto-grants-2006_11
特許番号
US07138530B2

反応ノート

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