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Hydrochloric Acid → HCID 21448657、化合物

HRID 596823
ノート
印刷プレビュー

反応式

HRID 596823 の反応式
[C:1]([C:3]1([CH2:18][CH2:19]Br)[C:9]2[CH:10]=[CH:11][CH:12]=[CH:13][C:8]=2[CH2:7][CH2:6][C:5]2[CH:14]=[CH:15][CH:16]=[CH:17][C:4]1=2)#[N:2].[ClH:21].[CH:22]12[CH2:29][CH2:28][CH:25]([CH2:26][CH2:27]1)[CH2:24][NH:23]2.C(=O)([O-])[O-].[K+].[K+].Cl>O.C(O)(C)C.C(OCC)C>[ClH:21].[C:1]([C:3]1([CH2:18][CH2:19][N:23]2[CH2:24][CH:25]3[CH2:28][CH2:29][CH:22]2[CH2:27][CH2:26]3)[C:9]2[CH:10]=[CH:11][CH:12]=[CH:13][C:8]=2[CH2:7][CH2:6][C:5]2[CH:14]=[CH:15][CH:16]=[CH:17][C:4]1=2)#[N:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 313Hydrochloric AcidHCID 11430Potassium CarbonateHCID 19088473HCID 19088473、化合物HCID 219848442-Azabicyclo[2.2.2]octane hydrochloride

生成物 1

HCID 21448657HCID 21448657、化合物

試薬・触媒・溶媒 3

HCID 962Water溶媒2 回
HCID 3283
Diethyl Ether
溶媒
HCID 3776Isopropanol溶媒

実験手順

A mixture of 6.5 parts 5-cyano-5-(2-bromoethyl)10,11-dihydro-5H-dibenzo[a,d]cycloheptene, 4.0 parts 2-azabicyclo[2.2.2]octane hydrochloride and 4.0 parts potassium carbonate in 88 parts N,N-dimethylsulfoxide and 20 parts water is heated at reflux for about 4 hours. After cooling, the reaction mixture is diluted with water, resulting in the formation of an oil. The water layer is decanted and the oil dissolved in ethyl ether. The ethereal solution is washed twice with water, once with a saturated sodium chloride solution, dried over anhydrous sodium sulfate and filtered. The solvent is removed to give an oil which is treated with a solution of hydrogen chloride in isopropanol. Addition of ethyl ether results in a precipitate that is separated, washed with ether and dried to afford-5-cyano-5[2-(2-azabicyclo[2.2.2]oct-2-yl)ethyl]-10,11-dihydro-5H-dibenzo[a,d]cycloheptene hydrochloride. This compound is represented by the following structural formula. ##STR14##

後処理

  1. temperatureis heated
  2. temperatureat reflux for about 4 hours
  3. temperatureAfter cooling
  4. customresulting in the formation of an oil
  5. customThe water layer is decanted
  6. dissolutionthe oil dissolved in ethyl ether
  7. washThe ethereal solution is washed twice with water, once with a saturated sodium chloride solution
  8. dry with materialdried over anhydrous sodium sulfate
  9. filtrationfiltered
  10. customThe solvent is removed
  11. customto give an oil which
  12. customresults in a precipitate that
  13. customis separated
  14. washwashed with ether
  15. customdried

出典と根拠

ORDレコード
ord-3fb9f6d6320d4adfbe98081382fc8a98
出典データセット
uspto-grants-1977_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04012393

反応ノート

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