Hydrochloric Acid → HCID 22506876、化合物

HRID 985601ノート

反応式

HRID 985601 の反応式
[I:1][CH2:2][C:3]1([CH3:21])[O:20][C:6]2=[C:7]([CH3:19])[C:8]3[CH2:9][C:10]([CH3:18])([CH3:17])[N:11](C=O)[C:12]=3[C:13]([CH3:14])=[C:5]2[CH2:4]1.Cl.C(=O)([O-])O.[Na+].O.C(OCC)(=O)C>CO>[I:1][CH2:2][C:3]1([CH3:21])[O:20][C:6]2=[C:7]([CH3:19])[C:8]3[CH2:9][C:10]([CH3:17])([CH3:18])[NH:11][C:12]=3[C:13]([CH3:14])=[C:5]2[CH2:4]1

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 516892Sodium BicarbonateHCID 22506878HCID 22506878、化合物HCID 22728543Water ethylacetate

生成物 1

HCID 22506876HCID 22506876、化合物収率 98%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a solution of 2,3,6,7-tetrahydro-2-(iodomethyl)-2,4,6,6,8-pentamethyl-5H-furo[2,3-f]indole-5-carbaldehyde (2.42 g, 6.06 mmol) in methanol (10 ml) was added concentrated hydrochloric acid (3 ml), and heated under reflux for 2.5 hours under nitrogen atmosphere. The reaction mixture was added dropwise to a mixture of sodium hydrogen carbonate (3.7 g, 44 mmol) with water-ethyl acetate, neutralized and extracted three times with ethyl acetate. The organic layers were combined, washed with water and saturated brine, dried over magnesium sulfate, filtered and concentrated under reduced pressure to obtain 2.20 g of the title compound.

後処理

  1. temperatureheated
  2. temperatureunder reflux for 2.5 hours under nitrogen atmosphere
  3. extractionextracted three times with ethyl acetate
  4. washwashed with water and saturated brine
  5. dry with materialdried over magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-aef4d9e3002e42e894949aeeef8b6547
出典データセット
uspto-grants-2005_03
特許番号
US06872718B1

反応ノート

読み込み中…