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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Water → Benfuresate

HRID 27643
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HRID 27643 반응식
S(Cl)(Cl)=O.[CH2:5]([S:7]([O:10][C:11]1[CH:16]=[CH:15][C:14](O)=[C:13]([C:18]([CH3:22])([CH3:21])[CH2:19][OH:20])[CH:12]=1)(=[O:9])=[O:8])[CH3:6].O>CN(C)C=O>[CH2:5]([S:7]([O:10][C:11]1[CH:16]=[CH:15][C:14]2[O:20][CH2:19][C:18]([CH3:22])([CH3:21])[C:13]=2[CH:12]=1)(=[O:9])=[O:8])[CH3:6]
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참가 물질

5

반응물 3

HCID 962WaterHCID 24386Thionyl ChlorideHCID 233412894-Hydroxy-3-(2-hydroxy-1,1-dimethylethyl)phenyl ethanesulphonate

생성물 1

HCID 3034378Benfuresate수율 69.9%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

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온도
5 °C

실험 절차

Thionyl chloride (4.3 g) was added dropwise to dimethylformamide (13 ml) maintained at about 5° C. To this was quickly added 4-hydroxy-3-(2-hydroxy-1,1-dimethylethyl)phenyl ethanesulphonate (9.5 g) from Example 2 in dimethylformamide (13 ml). The reaction mixture was then heated to 100° C. and maintained at that temperature for 4-5 hours, after which it was cooled and poured into water (100 ml). The oil was extracted with diethyl ether, washed with water, dried over magnesium sulphate and evaporated down to give 6.2 g of a brownish oil.

후처리

  1. temperatureThe reaction mixture was then heated to 100° C.
  2. temperaturemaintained at that temperature for 4-5 hours
  3. temperatureafter which it was cooled
  4. extractionThe oil was extracted with diethyl ether
  5. washwashed with water
  6. dry with materialdried over magnesium sulphate
  7. customevaporated down

출처 및 근거

ORD 기록
ord-3dae8ba852554d2e957caec290b2e483
출처 데이터셋
uspto-grants-1980_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04222767

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