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Water → HCID 70636775, 화합물

HRID 1658720
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HRID 1658720 반응식
[N:1]([CH:4]1[CH2:22][CH2:21][N:7]2[C:8]3[CH:20]=[CH:19][CH:18]=[CH:17][C:9]=3[CH2:10][C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=3[CH:6]2[CH2:5]1)=[N+]=[N-].[H-].[H-].[H-].[H-].[Li+].[Al+3].O>CCOCC.CO.CC(C)=O>[NH2:1][CH:4]1[CH2:22][CH2:21][N:7]2[C:8]3[CH:20]=[CH:19][CH:18]=[CH:17][C:9]=3[CH2:10][C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=3[CH:6]2[CH2:5]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 962WaterHCID 21226445Aluminium lithium hydrideHCID 86733598HCID 86733598, 화합물

생성물 1

HCID 70636775HCID 70636775, 화합물

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 21894497Aceton-methanol용매

실험 절차

4 g of 2-azido-1,2,3,4,10,14b-hexahydro-pyridino[1,2-a]-dibenzo[c,f]-azepine (axial) is added to a suspension of 3 g of LiAlH4 in dry ether. The mixture obtained is heated for 1 hour, and after that cooled down. Then 12 ml of water are added to the mixture dropwise, whereby an inorganic precipitate is formed. The inorganic residue is removed by filtration after which the filtrate is evaporated to dryness. Obtained in this manner: 3.5 g (oil). Rf in methanol:acetone (9:1) = 0.28 (axial position).

후처리

  1. customThe mixture obtained
  2. temperatureis heated for 1 hour
  3. temperatureafter that cooled down
  4. customwhereby an inorganic precipitate is formed
  5. customThe inorganic residue is removed by filtration after which the filtrate
  6. customis evaporated to dryness
  7. customObtained in this manner

출처 및 근거

ORD 기록
ord-e5d035d8afbc496d944121abb6b75976
출처 데이터셋
uspto-grants-1976_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03966723

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