N-bromobutanimide → tert-butyl (7-bromo-2-oxo-2,3,4,5-tetrahydro-1H-benzo[b]azepin-3-yl)carbamate

HRID 1670408ノート

反応式

HRID 1670408 の反応式
[Br:1]N1C(=O)CCC1=O.[O:9]=[C:10]1[CH:16]([NH:17][C:18](=[O:24])[O:19][C:20]([CH3:23])([CH3:22])[CH3:21])[CH2:15][CH2:14][C:13]2[CH:25]=[CH:26][CH:27]=[CH:28][C:12]=2[NH:11]1>CCOC(C)=O>[Br:1][C:26]1[CH:27]=[CH:28][C:12]2[NH:11][C:10](=[O:9])[CH:16]([NH:17][C:18](=[O:24])[O:19][C:20]([CH3:22])([CH3:23])[CH3:21])[CH2:15][CH2:14][C:13]=2[CH:25]=1

参加物

4

反応物 2

HCID 67184N-bromobutanimideHCID 13243501tert-butyl N-(2-oxo-2,3,4,5-tetrahydro-1H-1-benzazepin-3-yl)carbamate

生成物 1

HCID 57655892tert-butyl (7-bromo-2-oxo-2,3,4,5-tetrahydro-1H-benzo[b]azepin-3-yl)carbamate収率 203.3%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

472 mg of N-bromosuccinimide (2.65 mmol) are introduced at AT into a 100 ml round-bottomed flask, with stirring and under an argon atmosphere, containing 40 ml of EtOAc and 0.5 g of 2 (1.8 mmol). The medium is left stirring overnight, and is washed with 40 ml of HCl (1N), 40 ml of saturated aqueous solution of NaHCO3 and 40 ml of water. The organic phase is dried over MgSO4, filtered and then evaporated to dryness. 1.3 g of an oil are obtained, which oil is crystallized from 10 ml of isopropyl ether. After filter-drying, 450 mg of product 10 (white solid) are obtained.

後処理

  1. waitThe medium is left
  2. stirringstirring overnight
  3. washis washed with 40 ml of HCl (1N), 40 ml of saturated aqueous solution of NaHCO3 and 40 ml of water
  4. dry with materialThe organic phase is dried over MgSO4
  5. filtrationfiltered
  6. customevaporated to dryness

出典と根拠

ORDレコード
ord-01ba691965cd4403b1712313a19d21c5
出典データセット
uspto-grants-2011_08
特許番号
US07994162B2

反応ノート

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