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1,2-Dichloroethane → HCID 69932959, 화합물

HRID 540796
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HRID 540796 반응식
[F:1][C:2]([F:38])([F:37])[C:3]1[CH:36]=[CH:35][C:6]([O:7][C:8]2[N:12]([CH2:13][C:14](O)=[O:15])[N:11]=[C:10]([C:17]3[CH:22]=[CH:21][CH:20]=[C:19]([C:23]4([NH:27][C:28]([O:30][C:31]([CH3:34])([CH3:33])[CH3:32])=[O:29])[CH2:26][O:25][CH2:24]4)[CH:18]=3)[CH:9]=2)=[CH:5][CH:4]=1.Cl.[CH3:40][NH:41][CH3:42].C(Cl)CCl.C1C=CC2N(O)N=NC=2C=1.C(N(C(C)C)CC)(C)C>CN(C=O)C.CCOC(C)=O>[F:38][C:2]([F:1])([F:37])[C:3]1[CH:36]=[CH:35][C:6]([O:7][C:8]2[N:12]([CH2:13][C:14]([N:41]([CH3:42])[CH3:40])=[O:15])[N:11]=[C:10]([C:17]3[CH:18]=[C:19]([C:23]4([NH:27][C:28](=[O:29])[O:30][C:31]([CH3:32])([CH3:33])[CH3:34])[CH2:24][O:25][CH2:26]4)[CH:20]=[CH:21][CH:22]=3)[CH:9]=2)=[CH:5][CH:4]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 5

HCID 111,2-DichloroethaneHCID 10473Dimethylamine, hydrochlorideHCID 757711-HydroxybenzotriazoleHCID 81531DiisopropylethylamineHCID 67111333HCID 67111333, 화합물

생성물 1

HCID 69932959HCID 69932959, 화합물

시약·촉매·용매 2

HCID 6228
Dimethylformamide
용매
HCID 8857Ethyl Acetate용매

실험 절차

[5-(4-Trifluoromethylphenoxy)-3-(3-{3-[(tert-butyloxycarbonyl)amino]oxetan-3-yl}phenyl)-1H-pyrazol-1-yl]acetic acid (85 mg, 0.16 mmol), dimethylamine hydrochloride (26 mg, 0.32 mmol), EDC (46 mg, 0.24 mmol), HOBT (37 mg, 0.24 mmol), and diisopropylethylamine (0.11 mL, 0.64 mmol) were combined in 0.5 mL of DMF and the mixture was stirred at ambient temperature for 18 h. The mixture was diluted with EtOAc and washed with water and brine. The organic phase was dried over MgSO4, filtered, and the solvent was removed under reduced pressure. The residue was chromatographed on a 12 g silica gel column using 0-5% MeOH:CHCl3 over 15 min at 30 mL/min. Product-containing fractions were combined and the solvents were evaporated under reduced pressure to give tert-butyl [3-(3-{5-(4-trifluoromethylphenoxy)-1-[2-(dimethylamino)-2-oxoethyl]-1H-pyrazol-3-yl}phenyl)oxetan-3-yl]carbamate as a foam. Calcd (M+1)+: 561.6. Found: 561.0

후처리

  1. washwashed with water and brine
  2. dry with materialThe organic phase was dried over MgSO4
  3. filtrationfiltered
  4. customthe solvent was removed under reduced pressure
  5. customThe residue was chromatographed on a 12 g silica gel column
  6. waitCHCl3 over 15 min at 30 mL/min
  7. customthe solvents were evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-d754bcbfaf3e4cd4be3c72fcc25763ce
출처 데이터셋
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08871796B2

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