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Dichloromethane → Tert-butyl 4-(2-oxo-1,2-dihydroquinazolin-3(4H)-YL)piperidine-1-carboxylate

HRID 1172285
ノート
印刷プレビュー

反応式

HRID 1172285 の反応式
[N+:1]([C:4]1[CH:24]=[CH:23][CH:22]=[CH:21][C:5]=1[CH2:6][NH:7][CH:8]1[CH2:13][CH2:12][N:11]([C:14]([O:16][C:17]([CH3:20])([CH3:19])[CH3:18])=[O:15])[CH2:10][CH2:9]1)([O-])=O.C1N=CN([C:30](N2C=NC=C2)=[O:31])C=1.C(Cl)Cl.CCOC(C)=O>C1COCC1>[O:31]=[C:30]1[N:7]([CH:8]2[CH2:13][CH2:12][N:11]([C:14]([O:16][C:17]([CH3:20])([CH3:19])[CH3:18])=[O:15])[CH2:10][CH2:9]2)[CH2:6][C:5]2[C:4](=[CH:24][CH:23]=[CH:22][CH:21]=2)[NH:1]1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 6344DichloromethaneHCID 8857Ethyl AcetateHCID 682631,1'-CarbonyldiimidazoleHCID 13046886tert-Butyl 4-{[(2-nitrophenyl)methyl]amino}piperidine-1-carboxylate

生成物 1

HCID 53415303Tert-butyl 4-(2-oxo-1,2-dihydroquinazolin-3(4H)-YL)piperidine-1-carboxylate収率 24.4%

試薬・触媒・溶媒 1

HCID 8028
Tetrahydrofuran
溶媒
2 回

実験手順

To a solution of tert-butyl 4-(2-nitrobenzylamino)piperidine-1-carboxylate (13.2 g, 43.2 mmol) in THF (400 ml) was added a solution of CDI (7.7 g, 47.5 mmol) in 1:1 DCM: THF (100 ml) dropwise over 1 hour followed by stirring the reaction mixture for a further 16 hours. The reaction mixture was evaporated to give an oil that, when treated with EtOAc, precipitated the desired product. The precipitate was washed with cold EtOAc and dried to give a yellow solid (3.5 g). LC/MS (10% to 99%): M/Z (M+H)+ (obs)=332; tR=3.01.

後処理

  1. customThe reaction mixture was evaporated
  2. customto give an oil that, when
  3. customprecipitated the desired product
  4. washThe precipitate was washed with cold EtOAc
  5. customdried

出典と根拠

ORDレコード
ord-09d3c9277dbd4306b846f92f6906310a
出典データセット
uspto-grants-2010_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07834000B2

反応ノート

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