HCID 23002992、化合物 → 7-Chloro-8-morpholin-4-yl-2,3,4,5-tetrahydropyrido[3,2-f][1,4]oxazepine monohydrobromide

HRID 1692607ノート

反応式

HRID 1692607 の反応式
[Cl:1][C:2]1[C:12]([N:13]2[CH2:18][CH2:17][O:16][CH2:15][CH2:14]2)=[N:11][C:10]2[O:9][CH2:8][CH2:7][N:6](C(OC(C)(C)C)=O)[CH2:5][C:4]=2[CH:3]=1.[BrH:26].C(O)C>C(O)C>[BrH:26].[Cl:1][C:2]1[C:12]([N:13]2[CH2:14][CH2:15][O:16][CH2:17][CH2:18]2)=[N:11][C:10]2[O:9][CH2:8][CH2:7][NH:6][CH2:5][C:4]=2[CH:3]=1

参加物

4

反応物 2

HCID 23002992HCID 23002992、化合物HCID 67279788tert-butyl 7-chloro-8-morpholin-4-yl-2,3-dihydropyrido[3,2-f][1,4]oxazepine-4(5H)-carboxylate

生成物 1

HCID 672802287-Chloro-8-morpholin-4-yl-2,3,4,5-tetrahydropyrido[3,2-f][1,4]oxazepine monohydrobromide収率 25%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a solution of the compound (0.10 g) obtained in step 1 in ethanol (1 mL) was added hydrobromic acid-ethanol solution (1 mL), and the mixture was stirred at room temperature for 4 hr. The solvent was evaporated under reduced pressure, and the aqueous layer was made basic with ethyl acetate and aqueous sodium hydroxide solution. The organic layer was washed with brine and dried, and the solvent was evaporated under reduced pressure. Ethyl acetate was added to the residue, and hydrobromic acid-ethanol solution was added. The precipitate was collected by filtration to give the title compound (0.03 g, 25%) as a white powder.

後処理

  1. customThe solvent was evaporated under reduced pressure
  2. washThe organic layer was washed with brine
  3. customdried
  4. customthe solvent was evaporated under reduced pressure
  5. additionEthyl acetate was added to the residue, and hydrobromic acid-ethanol solution
  6. additionwas added
  7. filtrationThe precipitate was collected by filtration

出典と根拠

ORDレコード
ord-46e55518a98a4a57b21a3df181202d8b
出典データセット
uspto-grants-2012_04
特許番号
US08158617B2

反応ノート

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