Dabco → HCID 13753213, 화합물

HRID 1732154노트

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HRID 1732154 반응식
N12CCN(CC1)CC2.[CH2:9]([N:11]=[C:12]=[S:13])[CH3:10].[F:14][C:15]1[CH:31]=[CH:30][C:18]([O:19][C:20]2[CH:29]=[CH:28][C:23]([O:24][CH2:25][CH2:26][OH:27])=[CH:22][CH:21]=2)=[CH:17][CH:16]=1>N1C=CC=CC=1>[F:14][C:15]1[CH:31]=[CH:30][C:18]([O:19][C:20]2[CH:29]=[CH:28][C:23]([O:24][CH2:25][CH2:26][O:27][C:12](=[S:13])[NH:11][CH2:9][CH3:10])=[CH:22][CH:21]=2)=[CH:17][CH:16]=1

참가 물질

5

반응물 3

HCID 9237DabcoHCID 10966Ethyl isothiocyanateHCID 13753176HCID 13753176, 화합물

생성물 1

HCID 13753213HCID 13753213, 화합물

시약·촉매·용매 1

HCID 1049Pyridine용매

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온도
80 °C

실험 절차

50 mg of 1,4-diazabicyclo(2,2,2)octane and 0.9 g of ethyl isothiocyanate are added to a solution of 2.3 g of 2-[p-(p-fluorophenoxy)phenoxy]-ethanol in 10 ml of pyridine. The mixture is then allowed to stir at 80° C. for 16 hours. The cooled mixture is poured into 50 ml of ice/water and extracted three times with 80 ml of ethyl acetate each time. The extracts are washed twice with 50 ml of water each time and with 50 ml of sodium chloride solution. The extracts are dried over anhydrous sodium sulfate and evaporated. The residue is purified chromatography on silica gel with n-hexane/ethyl acetate (2:1) to yield pure [2-[p-(p-fluorophenoxy)phenoxy]-ethyl]N-ethylthiocarbamate; m.p. 73°-75° C.

후처리

  1. extractionextracted three times with 80 ml of ethyl acetate each time
  2. washThe extracts are washed twice with 50 ml of water each time
  3. dry with materialThe extracts are dried over anhydrous sodium sulfate
  4. customevaporated
  5. customThe residue is purified chromatography on silica gel with n-hexane/ethyl acetate (2:1)

출처 및 근거

ORD 기록
ord-05ceffc3e0b54e6f9ab6e7d38d13c0ed
출처 데이터셋
uspto-grants-1986_11
특허 번호
US04625048

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