Ammonium Hydroxide → HCID 178511888、化合物

HRID 2296619ノート

反応式

HRID 2296619 の反応式
Cl.[O:2]1[C:8]2[CH:9]=[CH:10][C:11]([NH2:13])=[CH:12][C:7]=2[CH2:6][NH:5][CH2:4][CH2:3]1.I.[S:15]1[CH:19]=[CH:18][C:17]([C:20](SC)=[NH:21])=[CH:16]1.[OH-].[NH4+]>C(O)C.O>[O:2]1[C:8]2[CH:9]=[CH:10][C:11]([NH:13][C:20]([C:17]3[CH:18]=[CH:19][S:15][CH:16]=3)=[NH:21])=[CH:12][C:7]=2[CH2:6][NH:5][CH2:4][CH2:3]1

参加物

6

反応物 3

HCID 14923Ammonium HydroxideHCID 18387495HCID 18387495、化合物HCID 131722237HCID 131722237、化合物

生成物 1

HCID 178511888HCID 178511888、化合物収率 22.1%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

2,3,4,5-Tetrahydro-1,4-benzoxazepin-7-ylamine hydrochloride (1.84 g, 8.4 mmol) was dissolved in 95% ethanol (40 ml) and 3-thiophenecarboximidothioic acid, methyl ester, hydroiodide (2.85 g, 10 mmol) was added. The mixture was stirred at room temperature for 2 days and then heated at 60° C. overnight and cooled. The solid (1.02 g) was collected. The filtrate was evaporated and the residue treated with ethyl acetate. The resulting crystals were collected and combined with the solid obtained previously. They were dissolved in water (20 ml), basified with conc. ammonium hydroxide, and extracted with methylene chloride (3×30 ml). The organic extracts were washed with water, dried over magnesium sulfate, and concentrated to give a solid (0.508 g), m.p. 150-152° C.

後処理

  1. temperatureheated at 60° C. overnight
  2. temperaturecooled
  3. customThe solid (1.02 g) was collected
  4. customThe filtrate was evaporated
  5. additionthe residue treated with ethyl acetate
  6. customThe resulting crystals were collected
  7. customobtained previously
  8. extractionextracted with methylene chloride (3×30 ml)
  9. washThe organic extracts were washed with water
  10. dry with materialdried over magnesium sulfate
  11. concentrationconcentrated

出典と根拠

ORDレコード
ord-8c246586e3974b0fb63ec0a03b399b85
出典データセット
uspto-grants-2002_12
特許番号
US06489322B1

反応ノート

読み込み中…