Aluminum(III) Chloride → HCID 20197208, 화합물

HRID 652411노트

반응식

HRID 652411 반응식
[CH3:1][NH:2][CH:3]1[CH2:9][CH:8](O)[C:7]2[CH:11]=[CH:12][CH:13]=[CH:14][C:6]=2[O:5][CH2:4]1.[Cl-:15].[Cl-].[Cl-].[Al+3]>COCCOC>[ClH:15].[CH3:1][NH:2][CH:3]1[CH:9]=[CH:8][C:7]2[CH:11]=[CH:12][CH:13]=[CH:14][C:6]=2[O:5][CH2:4]1

참가 물질

4

반응물 2

HCID 6451240Aluminum(III) ChlorideHCID 13446113HCID 13446113, 화합물

생성물 1

HCID 20197208HCID 20197208, 화합물수율 89.9%

시약·촉매·용매 1

HCID 80711,2-Dimethoxyethane용매

실험 절차

1.93 g of 3-methylamino-2,3,4,5-tetrahydro-1-benzoxepin-5-ol were added to 25 ml of ethylene glycol dimethyl ether and reacted with 1.5 g aluminum trichloride while cooling with ice. Subsequently, the reaction mixture was heated for 18 hours at boiling temperature. Thereafter, the solvent was evaporated; the residue was dissolved in water, and the solution was reacted with diluted sodium hydroxide solution and extracted with methylene chloride. The methylene chloride extract was evaporated, and the 3-methylamino-2,3-dihydro-1-benzoxepine which remained as a residue was converted to its hydrochloride as described in Example 1, and this was recrystallized from a methanol/ether mixture. 1.9 g of 3-methylamino-2,3-dihydro-1-benzoxepine hydrochloride were obtained. Melting point: 168°-170 degrees C.

후처리

  1. temperaturewhile cooling with ice
  2. temperatureSubsequently, the reaction mixture was heated for 18 hours
  3. customThereafter, the solvent was evaporated
  4. dissolutionthe residue was dissolved in water
  5. customthe solution was reacted with diluted sodium hydroxide solution
  6. extractionextracted with methylene chloride
  7. extractionThe methylene chloride extract
  8. customwas evaporated
  9. customthis was recrystallized from a methanol/ether mixture

출처 및 근거

ORD 기록
ord-b768a3240fdd42c19359463685b28e1f
출처 데이터셋
uspto-grants-1987_06
특허 번호
US04672062

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