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Water → HCID 21538544, 화합물

HRID 1076895
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HRID 1076895 반응식
[Cl:1][CH2:2][CH2:3][CH2:4][C:5]([C:7]1[CH:20]=[CH:19][C:18]2[S:17][C:16]3[C:11](=[CH:12][C:13]([C:21](=[O:26])[CH2:22][CH2:23][CH2:24]Cl)=[CH:14][CH:15]=3)[CH2:10][C:9]=2[CH:8]=1)=[O:6].[I-].[K+].[NH:29]1[CH2:34][CH2:33][CH2:32][CH2:31][CH2:30]1.O>C(Cl)(Cl)Cl>[OH2:6].[ClH:1].[ClH:1].[N:29]1([CH2:2][CH2:3][CH2:4][C:5]([C:7]2[CH:20]=[CH:19][C:18]3[S:17][C:16]4[C:11](=[CH:12][C:13]([C:21](=[O:26])[CH2:22][CH2:23][CH2:24][N:29]5[CH2:34][CH2:33][CH2:32][CH2:31][CH2:30]5)=[CH:14][CH:15]=4)[CH2:10][C:9]=3[CH:8]=2)=[O:6])[CH2:34][CH2:33][CH2:32][CH2:31][CH2:30]1
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참가 물질

6

반응물 4

HCID 962WaterHCID 4875Potassium IodideHCID 8082PiperidineHCID 12340288HCID 12340288, 화합물

생성물 1

HCID 21538544HCID 21538544, 화합물

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

A mixture of 40.7 g (0.10 mole) of 2,7-bis(4-chlorobutyryl)-thioxanthene, 1 g of potassium iodide and 200 ml of piperidine was stirred and heated on a steam bath for 72 hours. Upon cooling the solution was poured into 1 liter of water. The oily product obtained was dissolved in chloroform, washed with water then saturated NaCl solution, dried over magnesium sulfate and filtered. The filtrate was evaporated to a small volume, cooled, acidified to Congo Red with ethereal HCl and filtered. The resulting solid was recrystallized several times from ethanol to give the desired product. M.P. 229°-231°C.

후처리

  1. temperatureheated on a steam bath for 72 hours
  2. temperatureUpon cooling the solution
  3. customThe oily product obtained
  4. washwashed with water
  5. dry with materialsaturated NaCl solution, dried over magnesium sulfate
  6. filtrationfiltered
  7. customThe filtrate was evaporated to a small volume
  8. temperaturecooled
  9. filtrationfiltered
  10. customThe resulting solid was recrystallized several times from ethanol

출처 및 근거

ORD 기록
ord-117f3f4742ad493da415670509eec0c4
출처 데이터셋
uspto-grants-1976_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03957988

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