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Triethylamine → HCID 178522149, 화합물

HRID 1094485
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HRID 1094485 반응식
[OH:1][C:2]1[N:7]=[CH:6][N:5]=[C:4]([CH2:8][C:9]2[CH:10]=[C:11]3[C:16](=[CH:17][CH:18]=2)[C:15]([C:19](O)=[O:20])=[CH:14][CH:13]=[CH:12]3)[CH:3]=1.[F:22][C:23]1[CH:29]=[CH:28][C:26]([NH2:27])=[CH:25][C:24]=1[C:30]([F:33])([F:32])[F:31].CCN(CC)CC.CCCP(=O)=O>CN(C1C=CN=CC=1)C.CN(C=O)C.[Cl-].[Na+].O.CCOC(C)=O.O>[F:22][C:23]1[CH:29]=[CH:28][C:26]([NH:27][C:19]([C:15]2[C:16]3[C:11](=[CH:10][C:9]([CH2:8][C:4]4[CH:3]=[C:2]([OH:1])[N:7]=[CH:6][N:5]=4)=[CH:18][CH:17]=3)[CH:12]=[CH:13][CH:14]=2)=[O:20])=[CH:25][C:24]=1[C:30]([F:31])([F:32])[F:33]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

10

반응물 4

HCID 8471TriethylamineHCID 753774-Fluoro-3-(trifluoromethyl)anilineHCID 16167369Propylphosphoric anhydrideHCID 178524206HCID 178524206, 화합물

생성물 1

HCID 178522149HCID 178522149, 화합물

시약·촉매·용매 5

HCID 142844-(Dimethylamino)pyridine촉매
HCID 962
Water
용매
HCID 6228Dimethylformamide용매
HCID 8857Ethyl Acetate용매
HCID 57417360Sodium chloride; water용매

실험 절차

345 mg (1.23 mMol) 6-(6-hydroxy-pyrimidin-4-ylmethyl)-naphthalene-1-carboxylic acid (Step 3.8), 193 μl (1.5 mMol) 4-fluoro-3-trifluoromethyl-aniline, 1.7 ml (12.3 mMol) Et3N and 63 mg (0.52 mMol) DMAP are dissolved in 10 ml of dry DMF. Then a solution of 1.45 ml (50% in DMF; 2.48 mMol) propylphosphonic anhydride is added. After 20 min, the reaction mixture is poured into water, brine and EtOAc. The separated aq. phase is extracted twice with EtOAc. The organic layers are washed with water and brine, dried (Na2SO4) and concentrated. Chromatography (Combi Flash; CH2Cl2→CH2Cl2/MeOH 1:19) gives the title compound: MS: [M+1]+=442; TLC (CH2Cl2/MeOH 1:9): Rf=0.37; 1H-NMR (DMSO-d6): δ ppm 12.43 (s, 1H), 10.92 (s, HN), 8.36 (m, 1H), 8.17 (d, 1H), 8.11 (m, 3H), 7.92 (s, 1H), 7.78 (d, 1H), 7.7-7.5 (m, 3H), 6.25 (s, 1H), 3.99 (s, H2C).

후처리

  1. extractionThe separated aq. phase is extracted twice with EtOAc
  2. washThe organic layers are washed with water and brine
  3. dry with materialdried (Na2SO4)
  4. concentrationconcentrated

출처 및 근거

ORD 기록
ord-d5ac67afc2c349a99ebb78871b723a9c
출처 데이터셋
uspto-grants-2012_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08133886B2

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