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Chlorosulfonic acid → 2-Butyl-2-ethylaziridine

HRID 1415881
ノート
印刷プレビュー

反応式

HRID 1415881 の反応式
[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]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

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

生成物 1

HCID 217099702-Butyl-2-ethylaziridine収率 73.1%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

反応条件

温度
2.5 °C

実験手順

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.

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート

後処理

  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

出典と根拠

ORDレコード
ord-5e6efa47dda049ca9a37794fd5587511
出典データセット
uspto-grants-1999_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05910494

反応ノート

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