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Triphenylphosphine → 3-Cyclopropyl-5,6,10,11-tetrahydro-8-methyl-benzo[g]pyrazino[1,2-a]indole fumarate

HRID 486595
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HRID 486595 반응식
[CH3:1][C:2]1[C:7]2=[CH:8][C:9]3[CH2:10][CH2:11][C:12]4[CH:18]=[C:17](OS(C(F)(F)F)(=O)=O)[CH:16]=[CH:15][C:13]=4[C:14]=3[N:6]2[CH2:5][CH2:4][N:3]=1.[Cl-].[Li+].C1(P([C:42]2[CH:47]=[CH:46]C=CC=2)C2C=CC=CC=2)C=CC=CC=1.C([Sn](CCCC)(CCCC)C1CC1)CCC.[C:64]([OH:71])(=[O:70])/[CH:65]=[CH:66]/[C:67]([OH:69])=[O:68]>CN(C)C=O.C(O)C.Cl[Pd](Cl)([P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)[P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1.C(Cl)Cl.CO.O>[C:64]([OH:71])(=[O:70])/[CH:65]=[CH:66]/[C:67]([OH:69])=[O:68].[CH:46]1([C:17]2[CH:16]=[CH:15][C:13]3[C:14]4[N:6]5[CH2:5][CH2:4][N:3]=[C:2]([CH3:1])[C:7]5=[CH:8][C:9]=4[CH2:10][CH2:11][C:12]=3[CH:18]=2)[CH2:47][CH2:42]1
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참가 물질

11

반응물 5

HCID 11776TriphenylphosphineHCID 433294Lithium ChlorideHCID 444972Fumaric AcidHCID 10947505CyclopropyltributylstannaneHCID 21803393Trifluoromethanesulphonic acid 5,6,10,11-tetrahydro-8-methyl-benzo[g]pyrazino[1,2-a]indol-3-yl ester

생성물 1

HCID 19095261
3-Cyclopropyl-5,6,10,11-tetrahydro-8-methyl-benzo[g]pyrazino[1,2-a]indole fumarate
수율 4%

시약·촉매·용매 5

HCID 178418476HCID 178418476, 화합물촉매HCID 702Ethanol용매2회HCID 962Water용매HCID 6228Dimethylformamide용매HCID 21226129Dichloromethane methanol용매

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온도
120 °C

실험 절차

Trifluoromethanesulphonic acid 5,6,10,11-tetrahydro-8-methyl-benzo[g]pyrazino[1,2-a]indol-3-yl-ester (2.0 g), 1.85 g of anhydrous lithium chloride, 0.44 g of bis(triphenylphosphine)palladium dichloride, 0.88 g of triphenylphosphine and 3.5 g of tri-n-butyl-cyclopropyltin were suspended in 25 ml of dimethylformamide under argon and heated to 120° C. for 6 h. while stirring. The reaction mixture was added to 500 ml of water and extracted once with 200 ml of ethyl acetate and twice with 100 ml of ethyl acetate each time. The ethyl acetate extracts were extracted four times with 2N hydrochloric acid (1×100 ml, 3×50 ml), the aqueous phases were combined, made basic with 120 ml of 28% sodium hydroxide solution and extracted three times with 100 ml of methylene chloride each time. The combined methylene chloride extracts were washed twice with 60 ml of saturated potassium fluoride solution each time and once with 500 ml of water. The organic phase was dried with MgSO4 and freed from solvent. The residue, 1.1 g of brown oil, was chromatographed on 60 g of aluminium oxide (neutral, III) with methylene chloride as the eluent. There was obtained 0.67 g of crude product which was again chromato-graphed on 8 g of silica gel with methylene chloride/methanol mixtures (50:1 to 20:1). The product, 0.14 g of brown oil, was dissolved in a 10-fold amount of ethanol and treated with 1.1 equivalents of a saturated solution of fumaric acid in ethanol. After concentration to a volume of about 1 ml and addition of 3 ml of ethyl acetate there separated 0.11 g of brown crystals which were recrystallized from 4 ml of isopropanol. There were obtained 50 mg (4%) of 3-cyclopropyl-5,6,10,11-tetrahydro-8-methyl-benzo[g]pyrazino[1,2-a]indole fumarate (1:1); m.pt.: 184°-187° C. (dec.).

후처리

  1. extractionextracted once with 200 ml of ethyl acetate and twice with 100 ml of ethyl acetate each time
  2. extractionThe ethyl acetate extracts were extracted four times with 2N hydrochloric acid (1×100 ml, 3×50 ml)
  3. extractionextracted three times with 100 ml of methylene chloride each time
  4. washThe combined methylene chloride extracts were washed twice with 60 ml of saturated potassium fluoride solution each time
  5. dry with materialThe organic phase was dried with MgSO4
  6. customThe residue, 1.1 g of brown oil, was chromatographed on 60 g of aluminium oxide (neutral, III) with methylene chloride as the eluent
  7. customThere was obtained 0.67 g of crude product which
  8. concentrationAfter concentration
  9. additionto a volume of about 1 ml and addition of 3 ml of ethyl acetate there separated 0.11 g of brown crystals which
  10. customwere recrystallized from 4 ml of isopropanol

출처 및 근거

ORD 기록
ord-df14f7d6c55648e483b973be76ffea3f
출처 데이터셋
uspto-grants-1994_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05292732

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