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HCID 68603211, 화합물 → HCID 178448603, 화합물

HRID 1454951
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HRID 1454951 반응식
[NH2:1][C:2]1[CH:42]=[CH:41][CH:40]=[CH:39][C:3]=1[CH2:4][NH:5][C:6](=O)[CH2:7][N:8]1[C:17](=[O:18])[C:16]2[N:15]([CH2:19][C:20]#[C:21][CH3:22])[C:14]([N:23]3[CH2:28][CH2:27][CH2:26][CH:25]([NH:29][C:30]([O:32][C:33]([CH3:36])([CH3:35])[CH3:34])=[O:31])[CH2:24]3)=[N:13][C:12]=2[N:11]([CH3:37])[C:9]1=[O:10]>C(O)(=O)C>[N:1]1[C:2]2[C:3](=[CH:39][CH:40]=[CH:41][CH:42]=2)[CH2:4][NH:5][C:6]=1[CH2:7][N:8]1[C:17](=[O:18])[C:16]2[N:15]([CH2:19][C:20]#[C:21][CH3:22])[C:14]([N:23]3[CH2:28][CH2:27][CH2:26][CH:25]([NH:29][C:30]([O:32][C:33]([CH3:36])([CH3:35])[CH3:34])=[O:31])[CH2:24]3)=[N:13][C:12]=2[N:11]([CH3:37])[C:9]1=[O:10]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 1

HCID 68603211HCID 68603211, 화합물

생성물 1

HCID 178448603HCID 178448603, 화합물

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

A mixture of 280 mg of 1-[2-(2-amino-benzylamino)-2-oxo-ethyl]-3-methyl-7-(2-butyn-1-yl)-8-[3-(tert.-butyloxycarbonyl-amino)-piperidin-1-yl]-xanthine and 4 ml glacial acetic acid is heated to boiling for two hours. Then the reaction mixture is evaporated down and the flask residue is purified through a column of aluminium oxide (activity stage III) with methylene chloride/ethyl acetate/methanol (5:5:0 to 5:4:1) as eluant. In addition to the desired 1-[(3,4-dihydro-quinazolin-2-yl)methyl]-3-methyl-7-(2-butyn-1-yl)-8-[3-(tert.-butyloxycarbonyl-amino)-piperidin-1-yl]-xanthine, deprotected 1-[(3,4-dihydro-quinazolin-2-yl)methyl]-3-methyl-7-(2-butyn-1-yl)-8-(3-amino-piperidin-1-yl)-xanthine is also obtained.

후처리

temperature
is heated
  • customThen the reaction mixture is evaporated down
  • customthe flask residue is purified through a column of aluminium oxide (activity stage III) with methylene chloride/ethyl acetate/methanol (5:5:0 to 5:4:1) as eluant
  • additionIn addition to the desired 1-[(3,4-dihydro-quinazolin-2-yl)methyl]-3-methyl-7-(2-butyn-1-yl)-8-[3-(tert.-butyloxycarbonyl-amino)-piperidin-1-yl]-xanthine, deprotected 1-[(3,4-dihydro-quinazolin-2-yl)methyl]-3-methyl-7-(2-butyn-1-yl)-8-(3-amino-piperidin-1-yl)-xanthine
  • customis also obtained
  • 출처 및 근거

    ORD 기록
    ord-9f3bf0c7926247bdb1a73985eb603332
    출처 데이터셋
    uspto-grants-2009_01
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US07482337B2

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