Water → 3-(Tritylamino)-2-azepanone

HRID 1269748

反応式

HRID 1269748 の反応式
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

参加物

6

反応物 4

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

生成物 1

HCID 147292183-(Tritylamino)-2-azepanone収率 69.4%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

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%).

後処理

  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)

出典と根拠

ORDレコード
ord-5248271c0b0346c89a291907fc79473c
出典データセット
uspto-grants-2007_04
特許番号
US07199147B2

関連ノート

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