Chlorosulfonic acid → 2-Butyl-2-ethylaziridine

HRID 398812노트

반응식

HRID 398812 반응식
[NH2:1][C:2]([CH2:9][CH3:10])([CH2:5][CH2:6][CH2:7][CH3:8])[CH2:3]O.ClS(O)(=O)=O>C(#N)C>[CH2:5]([C:2]1([CH2:9][CH3:10])[CH2:3][NH:1]1)[CH2:6][CH2:7][CH3:8]

참가 물질

4

반응물 2

HCID 24638Chlorosulfonic acidHCID 534210662-Amino-2-ethylhexan-1-ol

생성물 1

HCID 217099702-Butyl-2-ethylaziridine수율 73.1%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

Acetonitrile (150 ml) and the product from (e) (20.0 g) were mixed under nitrogen, cooled to 2°-3° C. and chlorosulphonic acid (16.0 g, Aldrich) was added dropwise keeping the temperature below 10° C. The coolant was removed and the slurry left to stir for 80 minutes at room temperature. The reaction was concentrated in vacuo and co-distilled with water (50 ml). 50% Aqueous sodium hydroxide (55.2 g) and water (50 ml) were added and the mixture was distilled at atomospheric pressure. The organic layer was collected from the distillate and dried with solid potassium hydroxide to give the desired product (12.8 g). 1H NMR consistent with proposed structure.

후처리

  1. temperaturecooled to 2°-3° C.
  2. customthe temperature below 10° C
  3. customThe coolant was removed
  4. waitthe slurry left
  5. concentrationThe reaction was concentrated in vacuo and co-distilled with water (50 ml)
  6. addition50% Aqueous sodium hydroxide (55.2 g) and water (50 ml) were added
  7. distillationthe mixture was distilled at atomospheric pressure
  8. distillationThe organic layer was collected from the distillate
  9. dry with materialdried with solid potassium hydroxide

출처 및 근거

ORD 기록
ord-a0d50442749a456d92c9e208b09d463e
출처 데이터셋
uspto-grants-1998_10
특허 번호
US05817652

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