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Potassium Hydroxide → HCID 86660365、化合物

HRID 713847
ノート
印刷プレビュー

反応式

HRID 713847 の反応式
C([O:3][CH:4]([C:28](=[O:50])[CH:29]=[CH:30][CH:31]=[CH:32][CH:33]=[CH:34][CH:35]=[CH:36][CH:37]=[CH:38][CH:39]=[CH:40][CH2:41][CH2:42][CH2:43][CH2:44][CH2:45][CH2:46][CH2:47][CH2:48][CH3:49])[C:5](=[O:27])[CH:6]=[CH:7][CH:8]=[CH:9][CH:10]=[CH:11][CH:12]=[CH:13][CH:14]=[CH:15][CH:16]=[CH:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH3:26])=O.[OH-].[K+]>CCO>[C:28]([CH:4]([C:5](=[O:27])[CH:6]=[CH:7][CH:8]=[CH:9][CH:10]=[CH:11][CH:12]=[CH:13][CH:14]=[CH:15][CH:16]=[CH:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH3:26])[OH:3])(=[O:50])[CH:29]=[CH:30][CH:31]=[CH:32][CH:33]=[CH:34][CH:35]=[CH:36][CH:37]=[CH:38][CH:39]=[CH:40][CH2:41][CH2:42][CH2:43][CH2:44][CH2:45][CH2:46][CH2:47][CH2:48][CH3:49]
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 14797Potassium HydroxideHCID 86660366HCID 86660366、化合物

生成物 1

HCID 86660365HCID 86660365、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

The above didocosahexaenoylmethyl formate (III, 1.38 g, 2.1 mmol) and KOH (300 mg) were stirred in 90% EtOH (70 mL) at room temperature under nitrogen for 90 min. Upon completion of the reaction, most of the solvent was evaporated. The resulting mixture was treated with 60 mL of 2M HCl solution. The aqueous phase was extracted with ether (2×75 mL). The combined ether extract was washed with water (2×50 mL), brine (50 mL), and dried over anhydrous MgSO4. Evaporation of the solvent gave 1.18 g of crude IV as yellowish oil. The crude product was purified by column chromatography on silica gel (230-400 mesh, 50 mL) eluted with 0-6% ethyl acetate gradient in hexanes. This gave 1.0 g of didocosahexaenoyl methanol (IV) as colourless oil.

後処理

  1. customUpon completion of the reaction
  2. custommost of the solvent was evaporated
  3. additionThe resulting mixture was treated with 60 mL of 2M HCl solution
  4. extractionThe aqueous phase was extracted with ether (2×75 mL)
  5. extractionThe combined ether extract
  6. washwas washed with water (2×50 mL), brine (50 mL)
  7. dry with materialdried over anhydrous MgSO4
  8. customEvaporation of the solvent

出典と根拠

ORDレコード
ord-efdf8c2144924c0ea1977504a06e97d1
出典データセット
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09186325B2

反応ノート

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