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Water → 1-[2-(4,5,10,11-tetrahydro-1H-dibenzo[a,d]cyclohepten-5-yl)ethyl]pyrrolidine

HRID 2308849
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HRID 2308849 반응식
[CH2:1]1[C:11]2[CH2:10][CH2:9][C:8]3[CH:12]=[CH:13][CH:14]=[CH:15][C:7]=3[CH:6]([CH2:16][CH2:17]OS(C3C=CC(C)=CC=3)(=O)=O)[C:5]=2[CH2:4][CH:3]=[CH:2]1.O.[NH:30]1[CH2:34][CH2:33][CH2:32][CH2:31]1>>[CH2:1]1[C:11]2[CH2:10][CH2:9][C:8]3[CH:12]=[CH:13][CH:14]=[CH:15][C:7]=3[CH:6]([CH2:16][CH2:17][N:30]3[CH2:34][CH2:33][CH2:32][CH2:31]3)[C:5]=2[CH2:4][CH:3]=[CH:2]1
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참가 물질

4

반응물 3

HCID 962WaterHCID 31268PyrrolidineHCID 867417722-(4,5,10,11-tetrahydro-1H-dibenzo[a,d]cyclohepten-5-yl)ethyl-p-toluenesulfonate

생성물 1

HCID 201879291-[2-(4,5,10,11-tetrahydro-1H-dibenzo[a,d]cyclohepten-5-yl)ethyl]pyrrolidine

실험 절차

A suspension of 59.8 g of 2-(4,5,10,11-tetrahydro-1H-dibenzo[a,d]cyclohepten-5-yl)ethyl-p-toluenesulfonate in 180 ml of pyrrolidine is stirred under argon at room temperature for 21 hours, subsequently poured into a mixture of ice and 300 ml of water and extracted twice with 1.2 l of distilled ether each time. The organic extracts are washed twice with 400 ml of water each time and a small amount of ice, combined, dried over magnesium sulfate and evaporated. The residue is taken up twice in 100 ml of dry toluene each time and the solutions obtained are in each case evaporated to dryness. There is obtained 1-[2-(4,5,10,11-tetrahydro-1H-dibenzo[a,d]cyclohepten-5-yl)ethyl]pyrrolidine in the form of an oil which crystallizes upon standing; m.p. 56°-57°. By recrystallization from pentane there is obtained product of melting point 62°.

후처리

  1. extractionextracted twice with 1.2 l of distilled ether each time
  2. washThe organic extracts are washed twice with 400 ml of water each time
  3. dry with materialdried over magnesium sulfate
  4. customevaporated
  5. customthe solutions obtained
  6. customevaporated to dryness

출처 및 근거

ORD 기록
ord-28e4e71d881f4a0e971703770adfcf97
출처 데이터셋
uspto-grants-1987_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04691040

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