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Potassium Iodide → 1-Pentanone, 1,1'-(9H-thioxanthene-2,7-diyl)bis(5-(diethylamino)-, dihydrochloride

HRID 1076897
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HRID 1076897 반응식
[Cl:1][CH2:2][CH2:3][CH2:4][CH2:5][C:6]([C:8]1[CH:21]=[CH:20][C:19]2[S:18][C:17]3[C:12](=[CH:13][C:14]([C:22](=[O:28])[CH2:23][CH2:24][CH2:25][CH2:26]Cl)=[CH:15][CH:16]=3)[CH2:11][C:10]=2[CH:9]=1)=[O:7].[I-].[K+].[CH2:31]([NH:33][CH2:34][CH3:35])[CH3:32]>O1CCCC1>[ClH:1].[ClH:1].[CH2:31]([N:33]([CH2:34][CH3:35])[CH2:2][CH2:3][CH2:4][CH2:5][C:6]([C:8]1[CH:21]=[CH:20][C:19]2[S:18][C:17]3[C:12](=[CH:13][C:14]([C:22](=[O:28])[CH2:23][CH2:24][CH2:25][CH2:26][N:33]([CH2:34][CH3:35])[CH2:31][CH3:32])=[CH:15][CH:16]=3)[CH2:11][C:10]=2[CH:9]=1)=[O:7])[CH3:32]
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참가 물질

5

반응물 3

HCID 4875Potassium IodideHCID 8021DiethylamineHCID 12340289HCID 12340289, 화합물

생성물 1

HCID 2168601-Pentanone, 1,1'-(9H-thioxanthene-2,7-diyl)bis(5-(diethylamino)-, dihydrochloride

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
106 °C

실험 절차

A mixture of 20 g (0.0046 mole) of 2,7-bis(5-chlorovaleryl)-thioxanthene, 2 g of potassium iodide, 150 ml of diethylamine and 250 ml of tetrahyrofuran was heated to 106°C. in a Paar bomb for 24 hours with stirring. Upon cooling, the solvent was evaporated, and the remaining material was dissolved in heptane and filtered. The solution was acidified with ethereal HCl and the resulting precipitate was recrystallized several times from methanol and ethyl acetate to give the desired product. M.P. 197.5°-199.5°C.

후처리

  1. temperatureUpon cooling
  2. customthe solvent was evaporated
  3. dissolutionthe remaining material was dissolved in heptane
  4. filtrationfiltered
  5. customthe resulting precipitate was recrystallized several times from methanol and ethyl acetate

출처 및 근거

ORD 기록
ord-1e53ffb71f4848ac9e83860db440e307
출처 데이터셋
uspto-grants-1976_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03957988

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