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1,2-Dichloroethane → HCID 178463834, 화합물

HRID 2044054
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HRID 2044054 반응식
[NH2:1][C@@H:2]1[CH2:7][CH2:6][CH2:5][N:4]([C:8]2[CH:16]=[CH:15][C:11]([C:12]([NH2:14])=[O:13])=[C:10]([NH:17][C:18]3[CH:23]=[CH:22][C:21]([N:24]([CH2:27][CH3:28])[CH2:25][CH3:26])=[CH:20][CH:19]=3)[N:9]=2)[CH2:3]1.[C:29]([C:33]1[CH:37]=[C:36]([C:38](O)=[O:39])[NH:35][N:34]=1)([CH3:32])([CH3:31])[CH3:30].C(Cl)CCl.C1C=CC2N(O)N=NC=2C=1.CCN(CC)CC>C1COCC1.C(Cl)Cl>[C:29]([C:33]1[CH:37]=[C:36]([C:38]([NH:1][C@@H:2]2[CH2:7][CH2:6][CH2:5][N:4]([C:8]3[CH:16]=[CH:15][C:11]([C:12]([NH2:14])=[O:13])=[C:10]([NH:17][C:18]4[CH:23]=[CH:22][C:21]([N:24]([CH2:27][CH3:28])[CH2:25][CH3:26])=[CH:20][CH:19]=4)[N:9]=3)[CH2:3]2)=[O:39])[NH:35][N:34]=1)([CH3:32])([CH3:30])[CH3:31]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 5

HCID 111,2-DichloroethaneHCID 8471TriethylamineHCID 757711-HydroxybenzotriazoleHCID 66832948(R)-6-(3-aminopiperidin-1-yl)-2-(4-(diethylamino)phenylamino)nicotinamideHCID 178441096HCID 178441096, 화합물

생성물 1

HCID 178463834HCID 178463834, 화합물수율 59%

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 8028Tetrahydrofuran용매

실험 절차

A solution of (R)-6-(3-aminopiperidin-1-yl)-2-(4-(diethylamino)phenylamino)nicotinamide (40 mg, 0.105 mmol), 3-tert-butyl-1H-pyrazole-5-carboxylic acid (21.11 mg, 0.125 mmol), EDC (30.1 mg, 0.157 mmol), HOBT (24.02 mg, 0.157 mmol), and Et3N (0.022 mL, 0.157 mmol) in THF (1 mL) was stirred at rt for 4 h. The reaction mixture was diluted with CH2Cl2, washed with satd. NaHCO3, and concentrated. The residue was purified by prep-HPLC. The product containing fractions were collected, basified with satd. Na2CO3, separated, and concentrated to give 33 mg of (R)-6-(3-(3-tert-butyl-1H-pyrazole-5-carboxamido) piperidin-1-yl)-2-(4-(diethylamino)phenylamino) nicotinamide as a yellow solid. LCMS: (M+H)+=533.30. 1H NMR (400 MHz, CDCl3) δ ppm 10.96 (1H, br. s.), 10.52 (1H, s), 7.44 (1H, d, J=8.79 Hz), 7.36 (2H, d, J=8.79 Hz), 7.06 (1 H, br. s.), 6.59 (2H, d, J=9.23 Hz), 6.00 (1H, d, J=8.79 Hz), 5.75 (1H, br. s.), 4.16-4.27 (1H, m), 3.82 (1H, br. s.), 3.58-3.72 (3H, m), 3.27 (4H, q, J=7.18 Hz), 1.86-1.96 (2H, m), 1.78 (1H, d, J=5.71 Hz), 1.62-1.70 (1H, m), 1.60 (2H, s), 1.33 (9H, s), 1.10 (6H, t, J=7.03 Hz).

후처리

  1. washwashed with satd
  2. concentrationNaHCO3, and concentrated
  3. customThe residue was purified by prep-HPLC
  4. additionThe product containing fractions
  5. customwere collected
  6. customNa2CO3, separated
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-63f7bf21030f4e41a60df03bab4380f7
출처 데이터셋
uspto-grants-2013_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08586751B2

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