Triethylamine → HCID 14044811, 화합물

HRID 1449505노트

반응식

HRID 1449505 반응식
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([SH:8])=[CH:4][CH:3]=1.C(N(CC)CC)C.[CH2:16](Br)[CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH3:22]>C(#N)C>[CH2:16]([S:8][C:5]1[CH:6]=[CH:7][C:2]([NH2:1])=[CH:3][CH:4]=1)[CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH3:22]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 123691-BromoheptaneHCID 145104-Aminothiophenol

생성물 1

HCID 14044811HCID 14044811, 화합물수율 57.6%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

In 100 ml of acetonitrile was dissolved 5.90 g of 4-aminothiophenol. To the solution were added 6.57 ml of triethylamine and 8.44 g of n-heptylbromide, followed by stirring at room temperature for 18 hours. The precipitated crystals were collected by filtration, followed by removing the solvent. To the residue was added water and the mixture was extracted with ethyl acetate. The extract was washed successively with 1N sodium hydroxide aqueous solution and saturated sodium chloride aqueous solution and dried over anhydrous potassium carbonate. After removing the solvent, the residue was purified by silica gel column chromatography using 50 g of silica gel and using chloroform as eluent to obtain 6.06 g of the titled compound.

후처리

  1. filtrationThe precipitated crystals were collected by filtration
  2. customby removing the solvent
  3. additionTo the residue was added water
  4. extractionthe mixture was extracted with ethyl acetate
  5. washThe extract was washed successively with 1N sodium hydroxide aqueous solution and saturated sodium chloride aqueous solution
  6. dry with materialdried over anhydrous potassium carbonate
  7. customAfter removing the solvent
  8. customthe residue was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-cd8396329b95413aae915d0d2526d1bc
출처 데이터셋
uspto-grants-1997_02
특허 번호
US05599813

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