Ammonium Hydroxide → HCID 178511888, 화합물

HRID 2296619노트

반응식

HRID 2296619 반응식
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

참가 물질

6

반응물 3

HCID 14923Ammonium HydroxideHCID 18387495HCID 18387495, 화합물HCID 131722237HCID 131722237, 화합물

생성물 1

HCID 178511888HCID 178511888, 화합물수율 22.1%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-8c246586e3974b0fb63ec0a03b399b85
출처 데이터셋
uspto-grants-2002_12
특허 번호
US06489322B1

반응 노트

불러오는 중…