Ethyl Acetate → trans-(7-chloro-2,3,4,14b-tetrahydro-1H-dibenzo[b,f]pyrido[1,2-d][1,4]oxazepin-1-yl)carbamic acid chloromethyl ester

HRID 16159

反応式

HRID 16159 の反応式
C(=O)(O)[O-].[Na+].[Cl:6][C:7]1[CH:26]=[CH:25][C:10]2[O:11][C:12]3[CH:24]=[CH:23][CH:22]=[CH:21][C:13]=3[C@@H:14]3[C@H:19]([NH2:20])[CH2:18][CH2:17][CH2:16][N:15]3[C:9]=2[CH:8]=1.Cl[C:28]([O:30][CH2:31][Cl:32])=[O:29].C(OCC)(=O)C>C(Cl)Cl>[Cl:32][CH2:31][O:30][C:28](=[O:29])[NH:20][C@H:19]1[C@@H:14]2[N:15]([C:9]3[CH:8]=[C:7]([Cl:6])[CH:26]=[CH:25][C:10]=3[O:11][C:12]3[CH:24]=[CH:23][CH:22]=[CH:21][C:13]=32)[CH2:16][CH2:17][CH2:18]1

参加物

6

反応物 4

HCID 8857Ethyl AcetateHCID 62754Chloromethyl chloroformateHCID 516892Sodium BicarbonateHCID 70883458trans-7-chloro-2,3,4,14b-tetrahydro-1H-dibenzo[b,f]pyrido[1,2-d][1,4]oxazepine-1-amine

生成物 1

HCID 86599867trans-(7-chloro-2,3,4,14b-tetrahydro-1H-dibenzo[b,f]pyrido[1,2-d][1,4]oxazepin-1-yl)carbamic acid chloromethyl ester収率 88%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

100 μL of saturated aq. sodium bicarbonate was added to trans-7-chloro-2,3,4,14b-tetrahydro-1H-dibenzo[b,f]pyrido[1,2-d][1,4]oxazepine-1-amine (9.5 mg, 0.03 mmol) and chloromethyl chloroformate (64.2 μL, 0.42 mmol) in 250 μL of CH2Cl2. The resulting mixture was stirred at room temperature for 18 h. Subsequently, ethyl acetate was added and the organic layer was washed with water, dried (Na2SO4) and evaporated to give trans-(7-chloro-2,3,4,14b-tetrahydro-1H-dibenzo[b,f]pyrido[1,2-d][1,4]oxazepin-1-yl)carbamic acid chloromethyl ester (9.9 mg, 88%). Data: (m/z)=393 (M+H)+.

後処理

  1. washthe organic layer was washed with water
  2. dry with materialdried (Na2SO4)
  3. customevaporated

出典と根拠

ORDレコード
ord-65d4b72cde144581bdaebd6c8dfe058f
出典データセット
uspto-grants-2010_06
特許番号
US07737136B2

関連ノート

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