Sodium Carbonate → HCID 69354035, 화합물

HRID 1271294노트

반응식

HRID 1271294 반응식
[C:1]1([C:7]2[N:8]=[CH:9][C:10]([SH:19])=[N:11][C:12]=2[C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C(=O)([O-])[O-].[Na+].[Na+].[C:26]([O:30][C:31](=[O:39])[CH2:32][O:33][CH2:34][CH2:35][CH2:36][CH2:37]Br)([CH3:29])([CH3:28])[CH3:27]>CC(C)=O>[C:26]([O:30][C:31](=[O:39])[CH2:32][O:33][CH2:34][CH2:35][CH2:36][CH2:37][S:19][C:10]1[CH:9]=[N:8][C:7]([C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)=[C:12]([C:13]2[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=2)[N:11]=1)([CH3:29])([CH3:28])[CH3:27]

참가 물질

5

반응물 3

HCID 10340Sodium CarbonateHCID 86592459Tert-butyl (4-bromobutyloxy)acetateHCID 178527736HCID 178527736, 화합물

생성물 1

HCID 69354035HCID 69354035, 화합물수율 82.2%

시약·촉매·용매 1

HCID 180Acetone용매2회

실험 절차

To a solution of 500 mg of 5,6-diphenyl-2-pyrazinethiol in 20 ml of acetone, 321 mg of sodium carbonate was added and a solution of 556 mg of 2-(4-bromobutyloxy)acetic acid tert-butyl ester in 2 ml of acetone was added dropwise while stirring under ice-cooling, followed by stirring at room temperature for 24 hours. The solvent was evaporated under reduced pressure, and then the residue was combined with water and extracted with ethyl acetate. The extract was washed with saturated brine and dried over anhydrous magnesium sulfate, and then the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography to obtain 701 mg of the desired compound as a pale yellow oily substance.

후처리

  1. temperaturecooling
  2. stirringby stirring at room temperature for 24 hours
  3. customThe solvent was evaporated under reduced pressure
  4. extractionextracted with ethyl acetate
  5. washThe extract was washed with saturated brine
  6. dry with materialdried over anhydrous magnesium sulfate
  7. customthe solvent was evaporated under reduced pressure
  8. customThe residue was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-af372978f39e4dca808c632b52ae72e2
출처 데이터셋
uspto-grants-2007_04
특허 번호
US07205302B2

반응 노트

불러오는 중…