N-Iodosuccinimide → HCID 67035019、化合物

HRID 2354093ノート

反応式

HRID 2354093 の反応式
[CH2:1]=[C:2]1[CH2:7][CH2:6][CH:5]([OH:8])[CH2:4][CH2:3]1.[I:9]N1C(=O)CCC1=O>C(Cl)Cl>[I:9][CH2:1][C:2]12[O:8][CH:5]([CH2:6][CH2:7]1)[CH2:4][CH2:3]2

参加物

4

反応物 2

HCID 120273N-IodosuccinimideHCID 138082884-methylenecyclohexanol

生成物 1

HCID 67035019HCID 67035019、化合物収率 37.6%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of 4-methylenecyclohexanol (1.88 g) in CH2Cl2 (37.6 mL) was added N-iodosuccinimide (4.5 g) under nitrogen atmosphere, which was stirred at ambient temperature for 3 hours. The resultant was washed with Na2S2O3 aq., H2O, and brine. The organic phase was dried over Na2SO4, filtered, and evaporated in vacuo. The residue was purified by column chromatography on silica gel to give 1-(iodomethyl)-7-oxabicyclo[2.2.1]heptane (1.5 g) as colorless oil.

後処理

  1. washThe resultant was washed with Na2S2O3 aq., H2O, and brine
  2. dry with materialThe organic phase was dried over Na2SO4
  3. filtrationfiltered
  4. customevaporated in vacuo
  5. customThe residue was purified by column chromatography on silica gel

出典と根拠

ORDレコード
ord-c3bf2cdcacfb4b2db56473b55a35f981
出典データセット
uspto-grants-2010_07
特許番号
US07750155B2

反応ノート

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