3-(Methoxymethyl)-4-(2-methylpiperidin-1-yl)benzoic acid → HCID 67529400、化合物

HRID 219987ノート

反応式

HRID 219987 の反応式
[CH3:1][O:2][CH2:3][C:4]1[CH:5]=[C:6]([CH:10]=[CH:11][C:12]=1[N:13]1[CH2:18][CH2:17][CH2:16][CH2:15][CH:14]1[CH3:19])[C:7]([OH:9])=O.[NH2:20][C:21](=[N:37]O)[C:22]1[CH:23]=[C:24]([CH:34]=[CH:35][CH:36]=1)[O:25][CH2:26][CH2:27][CH2:28][C:29]([O:31][CH2:32][CH3:33])=[O:30]>>[CH3:1][O:2][CH2:3][C:4]1[CH:5]=[C:6]([C:7]2[O:9][N:37]=[C:21]([C:22]3[CH:23]=[C:24]([CH:34]=[CH:35][CH:36]=3)[O:25][CH2:26][CH2:27][CH2:28][C:29]([O:31][CH2:32][CH3:33])=[O:30])[N:20]=2)[CH:10]=[CH:11][C:12]=1[N:13]1[CH2:18][CH2:17][CH2:16][CH2:15][CH:14]1[CH3:19]

参加物

3

反応物 2

HCID 594958043-(Methoxymethyl)-4-(2-methylpiperidin-1-yl)benzoic acidHCID 72307492HCID 72307492、化合物

生成物 1

HCID 67529400HCID 67529400、化合物

実験手順

The title compound was prepared following procedure described for example 141, step 1, but starting from Intermediate 58 (158 mg; 0.60 mmol) and Intermediate 67 (151.79 mg; 0.57 mmol), the crude mixture was purified by flash chromatography (c-hex/(DCM/EtOAc 1:1) gradient from 1:0 to 1:1) to afford the title compound as a colorless oil. 1H NMR (CDCl3) δ 8.32 (d, J=2.1 Hz, 1H), 8.09 (dd, J=8.2, 2.1 Hz, 1H), 7.77 (dd, J=7.7, 1.2 Hz, 1H), 7.69 (dd, J=2.5, 1.4 Hz, 1H), 7.40 (t, J=8.0 Hz, 1H), 7.26 (d, J=8.3 Hz, 1H), 7.04 (ddd, J=8.3, 2.6, 0.9 Hz, 1H), 4.68-4.57 (m, 2H), 4.20-4.09 (m, 4H), 3.49 (s, 3H), 3.16 (br s, 1H), 3.06-3.02 (m, 1H), 2.65-2.62 (m, 1H), 2.56 (t, J=7.3 Hz, 2H), 2.20-2.11 (m, 2H), 1.86-1.69 (m, 4H), 1.49-1.45 (m, 2H), 1.27 (t, J=7.2 Hz, 3H), 0.89 (d, J=6.2 Hz, 3H). LC/MS (Method B): 494.5 (M+H)+. HPLC (Method A) Rt 4.59 min (Purity: 98.9%).

後処理

  1. customThe title compound was prepared following procedure
  2. customthe crude mixture was purified by flash chromatography (c-hex/(DCM/EtOAc 1:1) gradient from 1:0 to 1:1)

出典と根拠

ORDレコード
ord-5abd944d549a4d0bbeccb17ae133b6e6
出典データセット
uspto-grants-2012_06
特許番号
US08202865B2

反応ノート

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