Hydrochloric Acid → 4-Trifluoromethanesulfonylamino-butyryl chloride

HRID 723179노트

반응식

HRID 723179 반응식
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]

참가 물질

7

반응물 4

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

생성물 1

HCID 218861334-Trifluoromethanesulfonylamino-butyryl chloride

시약·촉매·용매 2

HCID 22350042dichloromethane N,N-dimethylformamide촉매HCID 887Methanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-f2eaef2f06b8454f8c501cc0c102a7c6
출처 데이터셋
uspto-grants-2006_11
특허 번호
US07138530B2

반응 노트

불러오는 중…