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Ethylenediamine → HCID 13279663, 화합물

HRID 1730976
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HRID 1730976 반응식
[C:1]([C:9]1[CH:17]=[CH:16][CH:15]=[CH:14][C:10]=1[C:11](O)=O)(=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH2:18]([NH2:21])[CH2:19][NH2:20].[Li].[H-]>O>[C:2]1([CH:1]2[C:9]3[CH:17]=[CH:16][CH:15]=[CH:14][C:10]=3[CH2:11][NH:21][CH2:18][CH2:19][NH:20]2)[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 3301EthylenediamineHCID 68132-Benzoylbenzoic AcidHCID 166653HydrideHCID 3028194Lithium

생성물 1

HCID 13279663HCID 13279663, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

Add 40 g. of the condensation product of o-benzoylbenzoic acid and ethylenediamine in small portions to a suspension of 15 g. of lithium aliminum hydride in 1500 ml. of anhydrous either with stirring. Reflux with stirring for 16 hours. Cool and add water carefully to decompose excess hydride. Separate the ether layer, dry over magnesium sulfate, and remove the solvent under reduced pressure to obtain 1,2,3,4,5,6-hexahydro-1-phenyl-2,5-benzodiazocine, m.p. 125° C. To prepare the dihydrochloride, dissolve the base in anhydrous ether and saturate with dry hydrogen chloride. Separate the precipitated solid, and recrystallize from ethanol to obtain 1,2,3,4,5,6-hexahydro-1-phenyl-2,5-benzodiazocine dihydrochloride, m.p. 297° C. (dec.).

후처리

  1. additionAdd 40 g
  2. temperatureReflux
  3. stirringwith stirring for 16 hours
  4. temperatureCool
  5. customSeparate the ether layer
  6. dry with materialdry over magnesium sulfate
  7. customremove the solvent under reduced pressure

출처 및 근거

ORD 기록
ord-d008aeb10f514019afa0db2c74350996
출처 데이터셋
uspto-grants-1976_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03994920

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