Sodium Hydroxide → 10,11-Dihydro-5-methyl-dibenzo[b,e][1,4]diazepine

HRID 2054143노트

반응식

HRID 2054143 반응식
[CH3:1][N:2]1[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=2[CH2:6][N:5](C(=O)C(F)(F)F)[C:4]2[CH:19]=[CH:20][CH:21]=[CH:22][C:3]1=2.[OH-].[Na+]>C(O)C>[CH3:1][N:2]1[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=2[CH2:6][NH:5][C:4]2[CH:19]=[CH:20][CH:21]=[CH:22][C:3]1=2

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 221352361-(10,11-Dihydro-5-methyl-dibenzo[b,e][1,4]diazepin-10-yl)-2,2,2-trifluoroethanone

생성물 1

HCID 2213523710,11-Dihydro-5-methyl-dibenzo[b,e][1,4]diazepine수율 94.7%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

1-(10,11-Dihydro-5-methyl-dibenzo[b,e][1,4]diazepin-10-yl)-2,2,2-trifluoroethanone of Step B (1.0 g) in ethanol (25 mL) was treated with 1 N sodium hydroxide (10 mL). The reaction mixture was refluxed for five hours, cooled, all volatiles removed in vacuo and the residue triturated with water. The resulting solid was filtered off, redissolved in dichloromethane and dried over anhydrous sodium sulfate. The solution was filtered through a short column of Magnesol® which was eluted with several additional volumes of dichloromethane. The total effluent was evaporated to dryness to provide the title compound as an off-white crystalline solid (0.65 g), m.p. 115-117° C.

후처리

  1. temperatureThe reaction mixture was refluxed for five hours
  2. temperaturecooled
  3. customall volatiles removed in vacuo
  4. customthe residue triturated with water
  5. filtrationThe resulting solid was filtered off
  6. dissolutionredissolved in dichloromethane
  7. dry with materialdried over anhydrous sodium sulfate
  8. filtrationThe solution was filtered through a short column of Magnesol® which
  9. washwas eluted with several additional volumes of dichloromethane
  10. customThe total effluent was evaporated to dryness

출처 및 근거

ORD 기록
ord-4d70bcf959aa474cad6d36367756485a
출처 데이터셋
uspto-grants-2008_02
특허 번호
US07329653B2

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