Dimethylcarbamoyl Chloride → HCID 13753208, 화합물

HRID 1732155노트

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HRID 1732155 반응식
[F:1][C:2]1[CH:18]=[CH:17][C:5]([O:6][C:7]2[CH:16]=[CH:15][C:10]([O:11][CH2:12][CH2:13][OH:14])=[CH:9][CH:8]=2)=[CH:4][CH:3]=1.[H-].[Na+].[CH3:21][N:22]([CH3:26])[C:23](Cl)=[O:24]>CN(C)C=O>[F:1][C:2]1[CH:18]=[CH:17][C:5]([O:6][C:7]2[CH:16]=[CH:15][C:10]([O:11][CH2:12][CH2:13][O:14][C:23](=[O:24])[N:22]([CH3:26])[CH3:21])=[CH:9][CH:8]=2)=[CH:4][CH:3]=1

참가 물질

5

반응물 3

HCID 6598Dimethylcarbamoyl ChlorideHCID 24758Sodium hydrideHCID 13753176HCID 13753176, 화합물

생성물 1

HCID 13753208HCID 13753208, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

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온도
40 °C

실험 절차

A solution of 2.5 g of 2-[p-(p-fluorophenoxy)phenoxy]-ethanol in 25 ml of dimethylformamide is added dropwise during 20 minutes while stirring to a suspension of 0.5 g of sodium hydride (55% in oil) in 5 ml of dimethylformamide. The mixture is then allowed to stir at 40° C. for 4 hours, then treated dropwise with 1.18 g of dimethylcarbamoyl chloride and allowed to react at 40° C. for 16 hours. The cooled mixture is poured into 75 ml of ice/water and extracted three times with 50 ml of ethyl acetate each time. The extracts are washed three times with 50 ml of water each time, dried and evaporated. The residue is purified by chromatography on silica gel with n-hexane/ethyl acetate (85:15) to yield pure [2-[p-(p-fluorophenoxy)phenoxy]-ethyl]N,N-dimethylcarbamate; nD20 =1.5444.

후처리

  1. customto react at 40° C. for 16 hours
  2. extractionextracted three times with 50 ml of ethyl acetate each time
  3. washThe extracts are washed three times with 50 ml of water each time
  4. customdried
  5. customevaporated
  6. customThe residue is purified by chromatography on silica gel with n-hexane/ethyl acetate (85:15)

출처 및 근거

ORD 기록
ord-c6163e5c6b234ee7b65d441e85bbb8d9
출처 데이터셋
uspto-grants-1986_11
특허 번호
US04625048

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