Triethylamine → Benzo[d]thiazol-3(2H)-yl(3,5-dichloro-4-methoxyphenyl)methanone

HRID 385005노트

반응식

HRID 385005 반응식
[S:1]1[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[NH:3][CH2:2]1.C(N(CC)CC)C.[Cl:17][C:18]1[CH:19]=[C:20]([CH:24]=[C:25]([Cl:29])[C:26]=1[O:27][CH3:28])[C:21](Cl)=[O:22]>C(Cl)(Cl)Cl>[Cl:17][C:18]1[CH:19]=[C:20]([CH:24]=[C:25]([Cl:29])[C:26]=1[O:27][CH3:28])[C:21]([N:3]1[C:4]2[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=2[S:1][CH2:2]1)=[O:22]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 96588BenzothiazolineHCID 38303153,5-Dichloro-4-methoxybenzoyl chloride

생성물 1

HCID 68109358Benzo[d]thiazol-3(2H)-yl(3,5-dichloro-4-methoxyphenyl)methanone

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

2,3-dihydro-1,3-benzothiazole was dissolved in chloroform (50 mL), and triethylamine (17.4 mL) and 3,5-dichloro-4-methoxybenzoyl chloride were added to the solution, and then the mixture was stirred at room temperature for 1 hour. The solvent was distilled off under reduced pressure and water was added, and then the mixture was extracted with ethyl acetate. The organic layer was washed with 1N hydrochloric acid, 1N sodium hydroxide and saturated brine, and then dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure and the obtained residue was used for the synthesis of (d).

후처리

  1. distillationThe solvent was distilled off under reduced pressure and water
  2. additionwas added
  3. extractionthe mixture was extracted with ethyl acetate
  4. washThe organic layer was washed with 1N hydrochloric acid, 1N sodium hydroxide and saturated brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. distillationThe solvent was distilled off under reduced pressure
  7. customthe obtained residue was used for the synthesis of (d)

출처 및 근거

ORD 기록
ord-e3b349571a4a4727933db1d119016147
출처 데이터셋
uspto-grants-2013_02
특허 번호
US08367843B2

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