Water → 3-(Tritylamino)-2-azepanone

HRID 1269748

반응식

HRID 1269748 반응식
C(N(CC)CC)C.[C:8]1([C:14](Cl)([C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)[C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.[NH2:28][CH:29]1[CH2:35][CH2:34][CH2:33][CH2:32][NH:31][C:30]1=[O:36].O>C(Cl)(Cl)Cl>[C:14]([NH:28][CH:29]1[CH2:35][CH2:34][CH2:33][CH2:32][NH:31][C:30]1=[O:36])([C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1)([C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 6456Trityl chlorideHCID 8471TriethylamineHCID 1024632H-Azepin-2-one, 3-aminohexahydro-

생성물 1

HCID 147292183-(Tritylamino)-2-azepanone수율 69.4%

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

Triethylamine (1.75 ml, 12.6 mmol) and triphenylmethyl chloride (3.50 g, 12.6 mmol) were added to a solution of 3-amino-2-azepanone (1.46 g, 11.4 mmol) in chloroform (44 ml) at room temperature and stirred overnight at room temperature. The reaction mixture was poured into water and then extracted with chloroform. The organic layer was washed with a saturated aqueous sodium chloride solution and then dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure and the resulting residue was purified by a silica gel column chromatography (eluent: chloroform/ethyl acetate) to obtain 3-(tritylamino)-2-azepanone (2.93 g, 69%).

후처리

  1. extractionextracted with chloroform
  2. washThe organic layer was washed with a saturated aqueous sodium chloride solution
  3. dry with materialdried over anhydrous magnesium sulfate
  4. distillationThe solvent was distilled off under reduced pressure
  5. customthe resulting residue was purified by a silica gel column chromatography (eluent: chloroform/ethyl acetate)

출처 및 근거

ORD 기록
ord-5248271c0b0346c89a291907fc79473c
출처 데이터셋
uspto-grants-2007_04
특허 번호
US07199147B2

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