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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
ノート
印刷プレビュー

反応式

HRID 863699 の反応式
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]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 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

生成物 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

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒2 回HCID 8857Ethyl Acetate溶媒2 回

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-b3e7a1f564b54424ae90a970405fc0c0
出典データセット
uspto-grants-1998_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05721245

反応ノート

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