Dabco → HCID 13753213、化合物

HRID 1732154ノート

反応式

HRID 1732154 の反応式
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

参加物

5

反応物 3

HCID 9237DabcoHCID 10966Ethyl isothiocyanateHCID 13753176HCID 13753176、化合物

生成物 1

HCID 13753213HCID 13753213、化合物

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

反応条件

温度
80 °C

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-05ceffc3e0b54e6f9ab6e7d38d13c0ed
出典データセット
uspto-grants-1986_11
特許番号
US04625048

反応ノート

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