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Hydrochloric Acid → 1,1,2-Tribromo-2-(2-hydroxyethyl)cyclopropane

HRID 1265984
ノート
印刷プレビュー

反応式

HRID 1265984 の反応式
[Br:1][C:2]1([Br:14])[CH2:4][C:3]1([Br:13])[CH2:5][CH2:6][O:7]C(OCC)C.O.C1(C)C=CC(S(O)(=O)=O)=CC=1.Cl>CO.O>[Br:1][C:2]1([Br:14])[CH2:4][C:3]1([Br:13])[CH2:5][CH2:6][OH:7]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 521998p-Toluenesulfonic acid monohydrateHCID 185481941,1,2-Tribromo-2-[2-(1-ethoxy-ethoxy)ethyl]-cyclopropane

生成物 1

HCID 185482081,1,2-Tribromo-2-(2-hydroxyethyl)cyclopropane収率 88.2%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962
Water
溶媒

実験手順

To a slurry of 16.5 g (0.0418 mol) of 1,1,2-tribromo-2-[2-(1-ethoxy-ethoxy)-ethyl]-cyclopropane in 145 ml methanol and 40 ml water, was added 0.306 g (0.00161 mol) p-toluene sulfonic acid monohydrate and 145 ml 6M hydrochloric acid. After stirring at room temperature for 1 hour, the solvent was removed from the reaction mixture in vacuo. To the residue, there was added ethyl acetate and water. The resulting mixture was transferred to a separatory funnel and the phases were separated. The isolated organic layer was washed with brine then dried over MgSO4 and filtered. The solvent was removed from the filtrate in vacuo to yield 11.9 g of 1,1,2-tribromo-2-(2-hydroxyethyl)cyclopropane as an oil.

後処理

  1. customthe solvent was removed from the reaction mixture in vacuo
  2. additionTo the residue, there was added ethyl acetate and water
  3. customThe resulting mixture was transferred to a separatory funnel
  4. customthe phases were separated
  5. washThe isolated organic layer was washed with brine
  6. dry with materialthen dried over MgSO4
  7. filtrationfiltered
  8. customThe solvent was removed from the filtrate in vacuo

出典と根拠

ORDレコード
ord-de6cfb93a6d846e8bd7627cee35c3a8d
出典データセット
uspto-grants-2003_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06548448B2

反応ノート

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