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1-Methylpiperazine → HCID 12945852, 화합물

HRID 325957
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HRID 325957 반응식
CN1CCNCC1.C1(S(NCCC2C=CC(CC(Cl)=O)=CC=2)(=O)=O)C=CC=CC=1.Cl.[CH3:31][N:32]1[CH2:37][CH2:36][N:35]([C:38](=[O:58])[CH2:39][C:40]2[CH:45]=[CH:44][C:43]([CH2:46][CH2:47][NH:48][S:49]([C:52]3[CH:57]=[CH:56][CH:55]=[CH:54][CH:53]=3)(=[O:51])=[O:50])=[CH:42][CH:41]=2)[CH2:34][CH2:33]1>N1C=CC=CC=1>[CH3:31][N:32]1[CH2:33][CH2:34][N:35]([C:38](=[O:58])[CH2:39][C:40]2[CH:41]=[CH:42][C:43]([CH2:46][CH2:47][NH:48][S:49]([C:52]3[CH:57]=[CH:56][CH:55]=[CH:54][CH:53]=3)(=[O:51])=[O:50])=[CH:44][CH:45]=2)[CH2:36][CH2:37]1
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참가 물질

5

반응물 3

HCID 531671-MethylpiperazineHCID 12945882HCID 12945882, 화합물HCID 131713489HCID 131713489, 화합물

생성물 1

HCID 12945852HCID 12945852, 화합물

시약·촉매·용매 1

HCID 1049Pyridine용매

반응 조건

온도
20 °C

실험 절차

To an ice-cooled solution of 3.0 g. (30 mmol) N-methylpiperazine and 100 ml. anhydrous pyridine are added portionwise, with stirring, in the course of one hour, 10.1 g. (30 mmol) 4-(2-benzenesulphonamidoethyl)-phenylacetyl chloride. Subsequently, the reaction mixture is allowed to warm up to 20° C., then heated for 5 hours at 90° C., cooled and poured into about 500 ml. ice water. The mixture is extracted with methylene chloride and the methylene chloride phase, after drying with anhydrous sodium sulphate, is evaporated. The residue is taken up in diethyl ether and the hydrochloride precipitated with ethereal hydrochloric acid. After recrystallization from ethanol, there are obtained 8.7 g. (66% of theory) 4-(2-benzenesulphonamidoethyl)-phenylacetic acid [4-methylpiperazide]hydrochloride; m.p. 168° C.

후처리

  1. temperatureheated for 5 hours at 90° C.
  2. temperaturecooled
  3. additionpoured into about 500 ml
  4. extractionThe mixture is extracted with methylene chloride
  5. dry with materialthe methylene chloride phase, after drying with anhydrous sodium sulphate
  6. customis evaporated
  7. customthe hydrochloride precipitated with ethereal hydrochloric acid
  8. customAfter recrystallization from ethanol, there
  9. customare obtained 8.7 g

출처 및 근거

ORD 기록
ord-dd4fcd0bd49f4510a8f38de02f9a5e52
출처 데이터셋
uspto-grants-1984_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04443477

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