Water → 2,3,4,5,11,15b-Hexahydro-2-methyl-1H-dibenz[3,4:6,7]azepino[1,2-a][1,4]diazepine

HRID 27889

반응식

HRID 27889 반응식
[CH3:1][NH:2][CH2:3][CH:4]1[NH:10][C:9]2[CH:11]=[CH:12][CH:13]=[CH:14][C:8]=2[CH2:7][C:6]2[CH:15]=[CH:16][CH:17]=[CH:18][C:5]1=2.C(N(CC)CC)C.O.Br[C:28](Br)([CH3:30])[CH3:29]>>[CH3:1][N:2]1[CH2:30][CH2:28][CH2:29][N:10]2[C:9]3[CH:11]=[CH:12][CH:13]=[CH:14][C:8]=3[CH2:7][C:6]3[CH:15]=[CH:16][CH:17]=[CH:18][C:5]=3[CH:4]2[CH2:3]1

참가 물질

5

반응물 4

HCID 962WaterHCID 8471TriethylamineHCID 116582,2-DibromopropaneHCID 130379126,11-Dihydro-N-methyl-5H-dibenz(b,e)azepine-6-methanamine

생성물 1

HCID 132010192,3,4,5,11,15b-Hexahydro-2-methyl-1H-dibenz[3,4:6,7]azepino[1,2-a][1,4]diazepine

실험 절차

4.76 g 5,6-dihydro-6-methylaminomethyl-11H-dibenzo[b,e]azepine is dissolved in 125 ml dibromopropane and 5 ml triethylamine is added to the solution. The mixture is boiled under reflux with stirring for 2 hours, after which it is cooled. 150 ml Water is then added and the whole is shaken for a little while, after which the aqueous layer is separated from the dibromopropane layer. The organic layer is subsequently dried over sodium sulphate and evaporated to dryness under vacuum. The residue is further purified chromatographically on a silica gel column with methanol:acetone (9:1) as eluent.

후처리

  1. temperatureunder reflux
  2. temperatureafter which it is cooled
  3. stirringthe whole is shaken for a little while
  4. customafter which the aqueous layer is separated from the dibromopropane layer
  5. dry with materialThe organic layer is subsequently dried over sodium sulphate
  6. customevaporated to dryness under vacuum
  7. customThe residue is further purified chromatographically on a silica gel column with methanol:acetone (9:1) as eluent

출처 및 근거

ORD 기록
ord-b9c6f2a81adb4f1a8cfe5312e711565d
출처 데이터셋
uspto-grants-1980_09
특허 번호
US04224321

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