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Methanol → alpha-Methylthio-alpha-(m-(2-phenyl-1,3-dioxa-2-cyclopentyl)phenyl)propionic acid

HRID 1277786
ノート
印刷プレビュー

反応式

HRID 1277786 の反応式
CO.[CH3:3][S:4][C:5]([C:11]1[CH:16]=[CH:15][CH:14]=[C:13]([C:17]2([C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=3)[O:21][CH2:20][CH2:19][O:18]2)[CH:12]=1)([CH3:10])[C:6]([O:8]C)=[O:7].[OH-].[Na+]>O>[CH3:3][S:4][C:5]([C:11]1[CH:16]=[CH:15][CH:14]=[C:13]([C:17]2([C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=3)[O:21][CH2:20][CH2:19][O:18]2)[CH:12]=1)([CH3:10])[C:6]([OH:8])=[O:7]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 887MethanolHCID 14798Sodium HydroxideHCID 12819455Methyl alpha-methylthio-alpha-[m-(2phenyl-1,3-dioxa-2-cyclopentyl)phenyl]propionate

生成物 1

HCID 12819458alpha-Methylthio-alpha-(m-(2-phenyl-1,3-dioxa-2-cyclopentyl)phenyl)propionic acid収率 97.7%

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

Methanol (4 ml) and 1 ml of water were added to 1.277 g of methyl α-methylthio-α-[m-(2-phenyl-1,3-dioxa-2-cyclopentyl)phenyl]propionate. Furthermore, 350 mg of sodium hydroxide was added, and the mixture was heated under reflux for 2 hours. After cooling, 30 ml of water was added, and the mixture was washed twice with 10 ml of diethyl ether. To the aqueous layer was added about 6 ml of 3.5% hydrochloric acid to adjust its pH to 3. It was then extracted four times with 20 ml of diethyl ether. The organic layer was washed twice with 10 ml of water, dried over anhydrous sodium sulfate, and evaporated under reduced pressure to afford 1.199 g of α-methylthio-α-[m-(2-phenyl-1,3-dioxa-2-cyclopentyl)phenyl]propionic acid as colorless crystals.

後処理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 2 hours
  3. temperatureAfter cooling
  4. washthe mixture was washed twice with 10 ml of diethyl ether
  5. additionTo the aqueous layer was added about 6 ml of 3.5% hydrochloric acid
  6. extractionIt was then extracted four times with 20 ml of diethyl ether
  7. washThe organic layer was washed twice with 10 ml of water
  8. dry with materialdried over anhydrous sodium sulfate
  9. customevaporated under reduced pressure

出典と根拠

ORDレコード
ord-9b27767a34df4042b446fab802844dd4
出典データセット
uspto-grants-1981_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04278802

反応ノート

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