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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Sodium Bicarbonate → HCID 22607995, 화합물

HRID 2080105
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HRID 2080105 반응식
[C:1]1([S:7][C:8]2[CH:9]=[C:10]([CH:14]3OCC[O:15]3)[CH:11]=[CH:12][CH:13]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C(=O)(O)[O-].[Na+]>C(O)C.O.O1CCCC1.S(=O)(=O)(O)O>[C:1]1([S:7][C:8]2[CH:9]=[C:10]([CH:11]=[CH:12][CH:13]=2)[CH:14]=[O:15])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 2

HCID 516892Sodium BicarbonateHCID 19421799HCID 19421799, 화합물

생성물 1

HCID 22607995HCID 22607995, 화합물수율 98%

시약·촉매·용매 4

HCID 702Ethanol용매HCID 962Water용매HCID 1118Sulfuric Acid용매
HCID 8028
Tetrahydrofuran
용매

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온도
0 °C

실험 절차

2-(3-Phenylsulfanyl-phenyl)-[1,3]dioxolane described in Preparation Example 91 (396 mg, 1.53 mmol) was dissolved in a mixture solution of ethanol (5 mL), water (5 mL), tetrahydrofuran (5 mL) and sulfuric acid (1 mL), and the solution was stirred for 2.5 hours under reflux. The reaction solution was cooled to 0° C., an aqueous solution of saturated sodium bicarbonate was added thereto, the solution was extracted with ethyl acetate, the organic layer was washed with brine and dried over anhydrous magnesium sulfate. The solvent was evaporated in vacuo, the residue was purified by silica gel column chromatography (hexane:ethyl acetate=20:1), and the title compound (323 mg, 1.51 mmol, 98%) was obtained as a colorless oil.

후처리

  1. temperatureunder reflux
  2. extractionthe solution was extracted with ethyl acetate
  3. washthe organic layer was washed with brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customThe solvent was evaporated in vacuo
  6. customthe residue was purified by silica gel column chromatography (hexane:ethyl acetate=20:1)

출처 및 근거

ORD 기록
ord-bc3a4863e7d949dc960214483889e6c6
출처 데이터셋
uspto-grants-2011_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07932272B2

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