Triethylamine → HCID 86645877, 화합물

HRID 2096805노트

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HRID 2096805 반응식
[Cl:1][C:2]1[N:11]=[C:10](Cl)[CH:9]=[CH:8][C:3]=1[C:4]([O:6][CH3:7])=[O:5].[Cl:13][C:14]1[CH:19]=[C:18]([OH:20])[CH:17]=[CH:16][C:15]=1[CH:21]([CH3:40])[C:22]([C:28]1[CH:39]=[CH:38][C:31]2[N:32]([CH3:37])[C:33](=[O:36])[N:34]([CH3:35])[C:30]=2[CH:29]=1)([OH:27])[C:23]([F:26])([F:25])[F:24].C(N(CC)CC)C.C1N2CCN(CC2)C1>CN(C=O)C.O>[CH3:7][O:6][C:4](=[O:5])[C:3]1[CH:8]=[CH:9][C:10]([O:20][C:18]2[CH:17]=[CH:16][C:15]([CH:21]([CH3:40])[C:22]([C:28]3[CH:39]=[CH:38][C:31]4[N:32]([CH3:37])[C:33](=[O:36])[N:34]([CH3:35])[C:30]=4[CH:29]=3)([OH:27])[C:23]([F:24])([F:25])[F:26])=[C:14]([Cl:13])[CH:19]=2)=[N:11][C:2]=1[Cl:1]

참가 물질

7

반응물 4

HCID 8471TriethylamineHCID 9237DabcoHCID 11106516Methyl 2,6-dichloropyridine-3-carboxylateHCID 59507321HCID 59507321, 화합물

생성물 1

HCID 86645877HCID 86645877, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

To a solution of methyl 2,6-dichloronicotinate (CAS Reg. No. 65515-28-8, 20 mg) in DMF (0.5 ml) was added 5-[2-(2-chloro-4-hydroxy-phenyl)-1-hydroxy-1-trifluoromethyl-propyl]-1,3-dimethyl-1,3-dihydro-benzoimidazol-2-one (Example 85, 40 mg), followed by triethyl amine (0.02 ml). The mixture was stirred for 10 min, then DABCO (2 mg) was added. The mixture was stirred at room temperature over night. Water was added to the mixture and extracted with EtOAc. The combined organic layers were dried over Na2SO4 and concentrated to an oil. The residue was purified by flash chromatography (SiO2, 1:2 EtOAc/heptane) to give the title compound (55 mg) as white foam. MS (m/e)=585.9 [M+H+].

후처리

  1. stirringThe mixture was stirred at room temperature over night
  2. extractionextracted with EtOAc
  3. dry with materialThe combined organic layers were dried over Na2SO4
  4. concentrationconcentrated to an oil
  5. customThe residue was purified by flash chromatography (SiO2, 1:2 EtOAc/heptane)

출처 및 근거

ORD 기록
ord-9c7a3c44a6304f32ab20285cb27939db
출처 데이터셋
uspto-grants-2013_05
특허 번호
US08450313B2

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