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1,2-Dichloroethane → HCID 178463834、化合物

HRID 2044054
ノート
印刷プレビュー

反応式

HRID 2044054 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

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

生成物 1

HCID 178463834HCID 178463834、化合物収率 59%

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-63f7bf21030f4e41a60df03bab4380f7
出典データセット
uspto-grants-2013_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08586751B2

反応ノート

読み込み中…

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