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Sodium methanethiolate → HCID 70976591, 화합물

HRID 514708
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HRID 514708 반응식
[CH3:1][S-:2].[Na+].Cl[CH2:5][C:6]1[CH:11]=[C:10]([N+:12]([O-:14])=[O:13])[CH:9]=[C:8]([F:15])[CH:7]=1>C(O)C.[Cl-].[Na+].O>[F:15][C:8]1[CH:9]=[C:10]([N+:12]([O-:14])=[O:13])[CH:11]=[C:6]([CH2:5][S:2][CH3:1])[CH:7]=1
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참가 물질

5

반응물 2

HCID 4378561Sodium methanethiolate2회HCID 569243861-(Chloromethyl)-3-fluoro-5-nitrobenzene

생성물 1

HCID 70976591HCID 70976591, 화합물수율 106.9%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 57417360Sodium chloride; water용매

실험 절차

Sodium methanethiolate (1.22 g; 17.4 mmol) was added in three portions to a stirred solution of 1-(chloromethyl)-3-fluoro-5-nitrobenzene (3.00 g; 15.8 mmol, HE Chemical) in ethanol (33 mL) at 0° C. The ice bath was removed and the batch was stirred at room temperature for 18 hours. Further sodium methanethiolate (0.33 g; 4.7 mmol) was added and the batch was stirred for 5 additional hours at room temperature. The batch was diluted with brine and extracted with ethyl acetate (2×). The combined organic phases were washed with water, dried (sodium sulfate), filtered and concentrated to give the desired product (3.4 g) that was used without further purification.

후처리

  1. customThe ice bath was removed
  2. stirringthe batch was stirred for 5 additional hours at room temperature
  3. extractionextracted with ethyl acetate (2×)
  4. washThe combined organic phases were washed with water
  5. dry with materialdried (sodium sulfate)
  6. filtrationfiltered
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-13917694c839425e94bd87acabf1c135
출처 데이터셋
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09108926B2

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