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1,2-Dichloroethane → 3-(2,4-Dichlorophenyl)-7-trifluoromethyl-imidazo[1,2-a]pyrimidine-6-carboxylic acid (tetrahydro-pyran-4-ylmethyl)-amide

HRID 229446
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HRID 229446 반응식
[OH-].[Na+].C(O[C:6]([C:8]1[C:9]([C:25]([F:28])([F:27])[F:26])=[N:10][C:11]2[N:12]([C:14]([C:17]3[CH:22]=[CH:21][C:20]([Cl:23])=[CH:19][C:18]=3[Cl:24])=[CH:15][N:16]=2)[CH:13]=1)=[O:7])C.C(Cl)CCl.C1[CH:34]=[CH:35][C:36]2N(O)N=[N:39][C:37]=2C=1.[O:43]1CCC[CH2:45][CH:44]1CN.C(N(CC)CC)C>C1COCC1.CO>[O:43]1[CH2:34][CH2:35][CH:36]([CH2:37][NH:39][C:6]([C:8]2[C:9]([C:25]([F:26])([F:27])[F:28])=[N:10][C:11]3[N:12]([C:14]([C:17]4[CH:22]=[CH:21][C:20]([Cl:23])=[CH:19][C:18]=4[Cl:24])=[CH:15][N:16]=3)[CH:13]=2)=[O:7])[CH2:45][CH2:44]1
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참가 물질

9

반응물 6

HCID 111,2-DichloroethaneHCID 8471TriethylamineHCID 14798Sodium HydroxideHCID 757711-HydroxybenzotriazoleHCID 97924(Tetrahydro-2H-pyran-2-ylmethyl)amineHCID 577584793-(2,4-Dichloro-phenyl)-7-trifluoromehyl-imidazo[1,2-a]pyrimidine-6-carboxylic acid ethyl ester

생성물 1

HCID 24748571
3-(2,4-Dichlorophenyl)-7-trifluoromethyl-imidazo[1,2-a]pyrimidine-6-carboxylic acid (tetrahydro-pyran-4-ylmethyl)-amide
수율 43%

시약·촉매·용매 2

HCID 887Methanol용매HCID 8028Tetrahydrofuran용매

실험 절차

Sodium hydroxide solution (2N, 0.3 mL) was added to 3-(2,4-dichloro-phenyl)-7-trifluoromehyl-imidazo[1,2-a]pyrimidine-6-carboxylic acid ethyl ester (113 mg, 0.28 mmol) in THF (1.2 mL) and methanol (0.3 mL) at room temperature. The resulting solution was stirred for 2 hours then concentrated to dryness. Ethyl acetate was added and removed in vacuo three times. The crude residue was diluted in DMF (1.5 mL) and EDC (3 eq, 0.84 mmol, 162 mg), HOBt (3 eq, 0.843 mmol, 114 mg) were added. The mixture was stirred for 15 minutes, then tetrahydropyran-methylamine (1.5 eq, 55 mg) and triethylamine (3 eq, 0.84 mmol, 0.12 mL) were added. The resulting mixture was stirred overnight. The reaction mixture was quenched by the addition of aqueous NH4Cl solution and the product was extracted with ethyl acetate. The crude product was purified using column chromatography (using 2% methanol/EtOAc as eluent) to afford 3-(2,4-dichlorophenyl)-7-trifluoromethyl-imidazo[1,2-a]pyrimidine-6-carboxylic acid (tetrahydro-pyran-4-ylmethyl)-amide in 43% yield. 1H NMR (DMSO-d6) δ 11.62 (1H), 8.54 (1H), 8.62 (1H), 8.41 (1H), 7.82 (1H), 7.60 (1H), 3.94 (2H), 3.72 (2H), 3.35 (2H), 1.98 (1H), 1.56 (2H), 1.34 (2H); m/z (M+H)=474.3.

후처리

  1. concentrationthen concentrated to dryness
  2. additionEthyl acetate was added
  3. customremoved in vacuo three times
  4. additionThe crude residue was diluted in DMF (1.5 mL)
  5. stirringThe mixture was stirred for 15 minutes
  6. stirringThe resulting mixture was stirred overnight
  7. customThe reaction mixture was quenched by the addition of aqueous NH4Cl solution
  8. extractionthe product was extracted with ethyl acetate
  9. customThe crude product was purified

출처 및 근거

ORD 기록
ord-9fd95b02953343478b06dddbc7f17c0b
출처 데이터셋
uspto-grants-2009_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07563797B2

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