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

HRID 27888
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반응식

HRID 27888 반응식
O=[C:2]1[CH2:8][CH2:7][N:6]2[C:9]3[CH:21]=[CH:20][CH:19]=[CH:18][C:10]=3[CH2:11][C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=3[CH:5]2[CH2:4][NH:3]1.O>C1COCC1>[CH2:4]1[NH:3][CH2:2][CH2:8][CH2:7][N:6]2[C:9]3[CH:21]=[CH:20][CH:19]=[CH:18][C:10]=3[CH2:11][C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=3[CH:5]12
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 962WaterHCID 233403572,3,4,5,11,15b-hexahydro-3-oxo-1H-dibenz[3,4:6,7]azepino[1,2-a](1,4)diazepine

생성물 1

HCID 132010182,3,4,5,11,15b-hexahydro-1H-dibenz[3,4:6,7]azepino[1,2-a](1,4)diazepine

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

반응 조건

온도
0 °C

실험 절차

A solution of 7.5 g 2,3,4,5,11,15b-hexahydro-3-oxo-1H-dibenz[3,4:6,7]azepino[1,2-a](1,4)diazepine in 200 ml THF is added to a vigorously stirred suspension of 5 g LiALH4 in 400 ml dry THF. The mixture is boiled under reflux for 3 hours, after which it is cooled to about 0° C. 20 ml water is then added slowly to the mixture and the inorganic precipitate which forms is removed by filtration. The filtrate is evaporated to dryness, leaving a crystalline residue. Yield 5.3 g.

후처리

  1. temperatureunder reflux for 3 hours
  2. customthe inorganic precipitate which forms is removed by filtration
  3. customThe filtrate is evaporated to dryness
  4. customleaving a crystalline residue

출처 및 근거

ORD 기록
ord-04490b33a97c443a8cb6ee4929ac67ce
출처 데이터셋
uspto-grants-1980_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04224321

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