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Hydrochloric Acid → 3-[6,7,8,9-tetrahydro-8-[(diisopropylamino)methyl]pyrido[1,2-a]indol-10-yl]-4-(1-methyl-3-indolyl)-1H-pyrrole-2,5-dione hydrochloride

HRID 863699
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인쇄 미리보기

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HRID 863699 반응식
C(O[CH2:5][CH:6]1[CH2:35][CH2:34][N:9]2[C:10]3[C:15]([C:16]([C:17]4[C:18](=O)[O:19][C:20](=[O:32])[C:21]=4[C:22]4[C:30]5[C:25](=[CH:26][CH:27]=[CH:28][CH:29]=5)[N:24]([CH3:31])[CH:23]=4)=[C:8]2[CH2:7]1)=[CH:14][CH:13]=[CH:12][CH:11]=3)(=O)C.[N:36]1C(C)=CC(C)=CC=1C.FC(F)(F)S(OS(C(F)(F)F)(=O)=O)(=O)=O.[CH:60]([NH:63][CH:64]([CH3:66])[CH3:65])([CH3:62])[CH3:61].[ClH:67]>ClCCl.C(OCC)(=O)C>[ClH:67].[CH:60]([N:63]([CH2:5][CH:6]1[CH2:35][CH2:34][N:9]2[C:10]3[C:15]([C:16]([C:17]4[C:18](=[O:19])[NH:36][C:20](=[O:32])[C:21]=4[C:22]4[C:30]5[C:25](=[CH:26][CH:27]=[CH:28][CH:29]=5)[N:24]([CH3:31])[CH:23]=4)=[C:8]2[CH2:7]1)=[CH:14][CH:13]=[CH:12][CH:11]=3)[CH:64]([CH3:66])[CH3:65])([CH3:62])[CH3:61]
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참가 물질

8

반응물 5

HCID 313Hydrochloric AcidHCID 7912DiisopropylamineHCID 79532,4,6-TrimethylpyridineHCID 67749Trifluoromethanesulfonic anhydrideHCID 103898823-[8-(Acetoxymethyl)-6,7,8,9-tetrahydropyrido[1,2-a]indol-10-yl]-4-(1-methyl-3-indolyl)furan-2,5-dione

생성물 1

HCID 19696352
3-[6,7,8,9-tetrahydro-8-[(diisopropylamino)methyl]pyrido[1,2-a]indol-10-yl]-4-(1-methyl-3-indolyl)-1H-pyrrole-2,5-dione hydrochloride

시약·촉매·용매 2

HCID 6344Dichloromethane용매2회HCID 8857Ethyl Acetate용매2회

실험 절차

A solution of 0.8 g of the product of Example 1 and 0.44 g of 2,4,6-collidine in 30 ml of dichloromethane was added to a solution of 0.9 g of trifluoromethanesulfonic anhydride in 10 ml of dichloromethane at 0° C. After 1.5 hour, the mixture was treated with 3.64 g of diisopropylamine and stirred for 16 hours. The mixture was washed with water and then with saturated aqueous sodium bicarbonate solution, dried and concentrated. The solid obtained was dissolved in ethyl acetate and treated wish a saturated solution of hydrogen chloride in ethyl acetate. Removal of the solvent in vacuo gave 260 mg of 3-[6,7,8,9-tetrahydro-8-[(diisopropylamino)methyl]pyrido[1,2-a]indol-10-yl]-4-(1-methyl-3-indolyl)-1H-pyrrole-2,5-dione hydrochloride of melting point 187° C. (decomposition).

후처리

  1. washThe mixture was washed with water
  2. dry with materialwith saturated aqueous sodium bicarbonate solution, dried
  3. concentrationconcentrated
  4. customThe solid obtained
  5. additiontreated
  6. customRemoval of the solvent in vacuo

출처 및 근거

ORD 기록
ord-b3e7a1f564b54424ae90a970405fc0c0
출처 데이터셋
uspto-grants-1998_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05721245

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