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2-n-Propyl-5-(2-aminoethyl)-3-[2'(1-trityl-1H-tetrazol-5-yl)biphenyl-4-yl]methylimidazole → HCID 178439974, 화합물

HRID 1655119
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HRID 1655119 반응식
[CH2:1]([C:4]1[N:5]([CH2:12][C:13]2[CH:18]=[CH:17][C:16]([C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][C:20]=3[C:25]3[N:29](C(C4C=CC=CC=4)(C4C=CC=CC=4)C4C=CC=CC=4)[N:28]=[N:27][N:26]=3)=[CH:15][CH:14]=2)[CH:6]=[C:7]([CH2:9][CH2:10][NH2:11])[N:8]=1)[CH2:2][CH3:3].O.[C:50]([O:54][CH2:55][CH3:56])(=[O:53])[CH:51]=[O:52].C([OH:59])C.Cl>O1CCCC1>[C:50]([OH:54])(=[O:53])[C:51]([OH:59])=[O:52].[CH2:1]([C:4]1[N:5]([CH2:12][C:13]2[CH:18]=[CH:17][C:16]([C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][C:20]=3[C:25]3[NH:29][N:28]=[N:27][N:26]=3)=[CH:15][CH:14]=2)[C:6]2[CH:51]([C:50]([O:54][CH2:55][CH3:56])=[O:53])[NH:11][CH2:10][CH2:9][C:7]=2[N:8]=1)[CH2:2][CH3:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 199329822-n-Propyl-5-(2-aminoethyl)-3-[2'(1-trityl-1H-tetrazol-5-yl)biphenyl-4-yl]methylimidazoleHCID 21887872Ethanol hydrochlorideHCID 22414697Ethyl glyoxylate hydrate

생성물 1

HCID 178439974HCID 178439974, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

To a mixture of 2-n-propyl-4-(2-aminoethyl)-1-[2'-(1-trityl-1H-tetrazol-5-yl)biphenyl-4-yl)methylimidazole (21.95 g) and tetrahydrofuran (200 ml) is added a solution of ethyl glyoxylate hydrate (4.25 g) in tetrahydrofuran (20 ml) at 5° C. The mixture is stirred overnight at room temperature and refluxed for 30 minutes. To a mixture is added a 8% hydrogen chloride ethanol solution (100 ml) at room temperature. The reaction mixture is stirred for 30 minutes, then evaporated. The residue is dissolved in chloroform and washed successively with a saturated sodium hydrogen carbonate solution and brine. The organic layer is dried and evaporated. The oxalate is recrystallized from ethanol to give ethyl 2-n-propyl-3-[2'-(1H-tetrazol-5-yl)biphenyl-4-yl]methyl-4,5,6,7-tetrahydroimidazo[4,5-c]pyridine-4-carboxylate oxalate (10.84 g).

후처리

  1. temperaturerefluxed for 30 minutes
  2. stirringThe reaction mixture is stirred for 30 minutes
  3. customevaporated
  4. dissolutionThe residue is dissolved in chloroform
  5. washwashed successively with a saturated sodium hydrogen carbonate solution and brine
  6. customThe organic layer is dried
  7. customevaporated
  8. customThe oxalate is recrystallized from ethanol

출처 및 근거

ORD 기록
ord-c9bc6ae52d6348d389c44eb2dddd1309
출처 데이터셋
uspto-grants-1995_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05409936

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