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

HRID 603915노트

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HRID 603915 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

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온도
0 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-0f1a9013a6d74f20a3f66234784ca979
출처 데이터셋
uspto-grants-2011_03
특허 번호
US07906502B2

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