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Chlorosulfonic acid → 2-Butyl-2-ethylaziridine

HRID 1415881
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HRID 1415881 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 물질반응 조건실험 절차후처리출처 및 근거반응 노트

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

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온도
2.5 °C

실험 절차

Acetonitrile (150 ml) and the product (20.0 g) from step (a) 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 atmospheric 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.

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후처리

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

출처 및 근거

ORD 기록
ord-5e6efa47dda049ca9a37794fd5587511
출처 데이터셋
uspto-grants-1999_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05910494

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