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Sodium Hydroxide → 7-(2,4,6-Triiodophenoxy)heptanoic acid

HRID 914644
ノート
印刷プレビュー

反応式

HRID 914644 の反応式
[I:1][C:2]1[CH:19]=[C:18]([I:20])[CH:17]=[C:16]([I:21])[C:3]=1[O:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][C:11]([O:13]CC)=[O:12].[OH-].[Na+]>C(O)C>[I:1][C:2]1[CH:19]=[C:18]([I:20])[CH:17]=[C:16]([I:21])[C:3]=1[O:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][C:11]([OH:13])=[O:12]
参加物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 14798Sodium HydroxideHCID 22939821Ethyl 7-(2,4,6-triiodophenoxy)heptanoate

生成物 1

HCID 229398227-(2,4,6-Triiodophenoxy)heptanoic acid収率 90%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

Ethanol (95%, 30 mL) was added with of ethyl 7-(2,4,6-triiodophenoxy)heptanoate (4.0 g) and the mixture was refluxed for dissolution, and the solution was added with sodium hydroxide (0.5 g) and further refluxed for 1.5 hours. The crystals obtained were separated by filtration, washed with ethanol and added with dichloromethane and 1 N hydrochloric acid to conduct extraction twice with dichloromethane. The organic layer was dried over anhydrous magnesium sulfate, and then the solvent was removed. The resulting residue was purified by silica gel column chromatography to obtain 7-(2,4,6-triiodophenoxy)heptanoic acid (3.4 g, yield: 90%).

後処理

  1. temperaturethe mixture was refluxed for dissolution
  2. temperaturefurther refluxed for 1.5 hours
  3. customThe crystals obtained
  4. customwere separated by filtration
  5. washwashed with ethanol
  6. additionadded with dichloromethane and 1 N hydrochloric acid
  7. extractionextraction twice with dichloromethane
  8. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  9. customthe solvent was removed
  10. customThe resulting residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-e21f11f741cf4ff3af753ba80f91ea69
出典データセット
uspto-grants-2007_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07264790B2

反応ノート

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