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2-Methyl-2-butene → HCID 67474068、化合物

HRID 2387751
ノート
印刷プレビュー

反応式

HRID 2387751 の反応式
CC(=CC)C.P([O-])(O)(O)=O.[Na+].Cl([O-])=[O:13].[Na+].[F:16][C:17]1[CH:18]=[C:19]([C@:23]2([CH2:28][O:29][C:30]3[C:35](=[O:36])[N:34]([CH2:37][O:38][CH3:39])[C:33]([CH3:40])=[N:32][C:31]=3[CH3:41])[CH2:25][C@H:24]2[CH:26]=[O:27])[CH:20]=[CH:21][CH:22]=1>C(Cl)(Cl)Cl.O.CC(C)=O.O>[F:16][C:17]1[CH:18]=[C:19]([C@:23]2([CH2:28][O:29][C:30]3[C:35](=[O:36])[N:34]([CH2:37][O:38][CH3:39])[C:33]([CH3:40])=[N:32][C:31]=3[CH3:41])[CH2:25][C@H:24]2[C:26]([OH:13])=[O:27])[CH:20]=[CH:21][CH:22]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 105532-Methyl-2-buteneHCID 23668197Sodium ChloriteHCID 23672064Monosodium phosphateHCID 87337461HCID 87337461、化合物

生成物 1

HCID 67474068HCID 67474068、化合物収率 100.1%

試薬・触媒・溶媒 3

HCID 962Water溶媒
HCID 6212
Chloroform
溶媒
HCID 18366337Propan-2-one--water (1/1)溶媒

実験手順

2-methyl 2-butene (1.14 ml), sodium dihydrogen phosphate (389 mg) and sodium chlorite (305 mg) were added to an acetone-water mixed solvent (8 ml-2 ml) of the compound 326-8 (779 mg). The obtained mixture was stirred at room temperature for 1 hour. Thereafter, water was added to the reaction solution, and chloroform was added to the reaction solution to carry out liquid separation and extraction. A small amount of 1 N hydrochloric acid was added to the obtained extract, and chloroform was further added to the reaction solution to carry out liquid separation and extraction. The obtained organic layer was dried over magnesium sulfate. The organic layer was dried over anhydrous magnesium sulfate and concentrated under reduced pressure, so as to obtain a crude product of the title carboxylic acid (814 mg).

後処理

  1. additionwas added to the reaction solution
  2. customliquid separation and extraction
  3. additionA small amount of 1 N hydrochloric acid was added to the obtained
  4. extractionextract
  5. additionchloroform was further added to the reaction solution
  6. customliquid separation and extraction
  7. dry with materialThe obtained organic layer was dried over magnesium sulfate
  8. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  9. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-19b186198e2a453a97bcd384826e235e
出典データセット
uspto-grants-2012_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08268848B2

反応ノート

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