Lithium Hydroxide → ({[2-(1,3-Benzodioxol-5-yl)-5,5-dimethyl-1,3-dioxan-2-yl]methyl}thio)acetic Acid

HRID 603915ノート

反応式

HRID 603915 の反応式
[O:1]1[C:5]2[CH:6]=[CH:7][C:8]([C:10]3([CH2:18][S:19][CH2:20][C:21]([O:23]CC)=[O:22])[O:15][CH2:14][C:13]([CH3:17])([CH3:16])[CH2:12][O:11]3)=[CH:9][C:4]=2[O:3][CH2:2]1.[Li+].[OH-]>O>[O:1]1[C:5]2[CH:6]=[CH:7][C:8]([C:10]3([CH2:18][S:19][CH2:20][C:21]([OH:23])=[O:22])[O:15][CH2:14][C:13]([CH3:17])([CH3:16])[CH2:12][O:11]3)=[CH:9][C:4]=2[O:3][CH2:2]1

参加物

4

反応物 2

HCID 3939Lithium HydroxideHCID 59197900Ethyl ({[2-(1,3-benzodioxol-5-yl)-5,5-dimethyl-1,3-dioxan-2-yl]methyl}thio)acetate

生成物 1

HCID 59197899({[2-(1,3-Benzodioxol-5-yl)-5,5-dimethyl-1,3-dioxan-2-yl]methyl}thio)acetic Acid

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
0 °C

実験手順

Ethyl ({[2-(1,3-benzodioxol-5-yl)-5,5-dimethyl-1,3-dioxan-2-yl]methyl}thio)acetate (Method 12) (14.2 g, 0.039 mol) was dissolved in THP (300 mL) and cooled to 0° C. LiOH (4.87 g, 0.12 mol) in water (100 mL) was added, and the mixture was given room temperature and stirred for 19 hours. The solvents were evaporated, the crude product was added water and extracted with diethyl ether. The aqueous layer was added 1M HCl until pH=3 and extracted twice with CH2Cl2. The combined CH2Cl2 layers were dried (Na2SO4) and concentrated under reduced pressure to afford the desired product.

後処理

  1. customwas given room temperature
  2. customThe solvents were evaporated
  3. additionthe crude product was added water
  4. extractionextracted with diethyl ether
  5. additionThe aqueous layer was added 1M HCl until pH=3
  6. extractionextracted twice with CH2Cl2
  7. dry with materialThe combined CH2Cl2 layers were dried (Na2SO4)
  8. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-0f1a9013a6d74f20a3f66234784ca979
出典データセット
uspto-grants-2011_03
特許番号
US07906502B2

反応ノート

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