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Triethylamine → (r)-5,11-Dihydro-5-(2-pyrrolidinylmethyl)dibenzo[b,e][1,4]oxazepine

HRID 411964
ノート
印刷プレビュー

反応式

HRID 411964 の反応式
Cl.O1CCOCC1.C(OC([N:15]1[CH2:19][CH2:18][CH2:17][C@@H:16]1[CH2:20][N:21]1[C:27]2[CH:28]=[CH:29][CH:30]=[CH:31][C:26]=2[CH2:25][O:24][C:23]2[CH:32]=[CH:33][CH:34]=[CH:35][C:22]1=2)=O)(C)(C)C.C(N(CC)CC)C>O1CCOCC1>[NH:15]1[CH2:19][CH2:18][CH2:17][C@@H:16]1[CH2:20][N:21]1[C:27]2[CH:28]=[CH:29][CH:30]=[CH:31][C:26]=2[CH2:25][O:24][C:23]2[CH:32]=[CH:33][CH:34]=[CH:35][C:22]1=2
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 8471TriethylamineHCID 204431481,4-Dioxane hydrochlorideHCID 69947237(r)-5,11-Dihydro-5-[1-(t-butoxycarbonyl)-2-pyrrolidinylmethyl]dibenzo[b,e][1,4]oxazepine

生成物 1

HCID 69200761(r)-5,11-Dihydro-5-(2-pyrrolidinylmethyl)dibenzo[b,e][1,4]oxazepine

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

4 M hydrochloride/dioxane solution (1.5 ml) was added to a solution of 400 mg of (R)-5,11-dihydro-5-[1-(t-butoxycarbonyl)-2-pyrrolidinylmethyl]dibenzo[b,e][1,4]oxazepine in dioxane (1.5 ml)), and the mixture was stirred at room temperature for one hour. The solvent was evaporated under reduced pressure. The residue was dissolved in dichloromethane (20 ml). Triethylamine (0.16 ml, 1.1 mmol) was added to the obtained solution, and the solution was stirred at room temperature for 30 minutes and then washed with saturated aqueous sodium bicarbonate solution. The organic layer was dried over magnesium sulfate. The solvent was evaporated under reduced pressure to obtain the title compound, i.e. (R)-5,11-dihydro-5-(2-pyrrolidinylmethyl)dibenzo [b,e][1,4]oxazepine, in the form of a light yellow oil(280 mg, 96%).

後処理

  1. customThe solvent was evaporated under reduced pressure
  2. dissolutionThe residue was dissolved in dichloromethane (20 ml)
  3. stirringthe solution was stirred at room temperature for 30 minutes
  4. washwashed with saturated aqueous sodium bicarbonate solution
  5. dry with materialThe organic layer was dried over magnesium sulfate
  6. customThe solvent was evaporated under reduced pressure

出典と根拠

ORDレコード
ord-9ab917076eae4a00a04f12091e7c133b
出典データセット
uspto-grants-2003_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06562808B1

反応ノート

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