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Triethylamine → 2-[2-fluoro-4-(2-{(1S,2R)-2-[1-(5-methoxypyrimidin-2-yl)piperidin-4-yl]cyclopropyl}ethoxy)phenyl]-1-(3-hydroxyazetidin-1-yl)ethanone

HRID 1474695
ノート
印刷プレビュー

反応式

HRID 1474695 の反応式
[F:1][C:2]1[CH:7]=[C:6]([O:8][CH2:9][CH2:10][C@@H:11]2[CH2:13][C@@H:12]2[CH:14]2[CH2:19][CH2:18][N:17]([C:20]3[N:25]=[CH:24][C:23]([O:26][CH3:27])=[CH:22][N:21]=3)[CH2:16][CH2:15]2)[CH:5]=[CH:4][C:3]=1[CH2:28][C:29](O)=[O:30].O.ON1C2C=CC=CC=2N=N1.Cl.[OH:44][CH:45]1[CH2:48][NH:47][CH2:46]1.Cl.C(/N=N/CCCN(C)C)C.C(N(CC)CC)C>C(Cl)Cl.CCOC(C)=O>[F:1][C:2]1[CH:7]=[C:6]([O:8][CH2:9][CH2:10][C@@H:11]2[CH2:13][C@@H:12]2[CH:14]2[CH2:15][CH2:16][N:17]([C:20]3[N:21]=[CH:22][C:23]([O:26][CH3:27])=[CH:24][N:25]=3)[CH2:18][CH2:19]2)[CH:5]=[CH:4][C:3]=1[CH2:28][C:29]([N:47]1[CH2:48][CH:45]([OH:44])[CH2:46]1)=[O:30]
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 8471TriethylamineHCID 27592903-Hydroxyazetidine hydrochlorideHCID 27960291-Hydroxybenzotriazole hydrateHCID 89583872[2-fluoro-4-(2-{(1S,2R)-2-[1-(5-methoxypyrimidin-2-yl)piperidin-4-yl]cyclopropyl}ethoxy)phenyl]acetic acidHCID 178465607HCID 178465607、化合物

生成物 1

HCID 89583861
2-[2-fluoro-4-(2-{(1S,2R)-2-[1-(5-methoxypyrimidin-2-yl)piperidin-4-yl]cyclopropyl}ethoxy)phenyl]-1-(3-hydroxyazetidin-1-yl)ethanone

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 8857Ethyl Acetate溶媒

実験手順

[2-Fluoro-4-(2-{(1S,2R)-2-[1-(5-methoxypyrimidin-2-yl)piperidin-4-yl]cyclopropyl}ethoxy)phenyl]acetic acid (80 mg, 0.186 mmol), 1-hydroxybenzotriazole hydrate (42.8 mg, 0.279 mmol), 3-hydroxyazetidine hydrochloride (30.6 mg, 0.279 mmol) and (E)-3-(ethyldiazenyl)-N,N-dimethylpropan-1-amine hydrochloride (50.2 mg, 0.279 mmol) were dissolved in CH2Cl2 (4 ml). The mixture was stirred at RT for 5 min. and triethylamine (0.078 ml, 0.556 mmol) was added. The mixture was stirred at RT overnight and loaded directly on Preparative TLC that was developed with pure EtOAc. The desired product (Rf=0.35 @ pure EtOAc) was collected to give the title compound. 1H NMR (500 MHz, CDCl3) δ 8.1 (s, 2H), 7.21 (m, 1H), 6.65 (m, 2H), 4.60 (m, 3H), 4.30 (m, 2H), 4.05 (m, 3H), 3.90 (m, 1H), 3.80 (s, 3H), 3.72 (s, broad, 1H), 3.41 (s, 2H), 2.83 (m, 2H), 2.15 (m, 1H), 2.05 (s, broad, 1H), 1.92 (m, 2H), 1.55 (m, 1H), 1.40 (m, 2H), 0.95 (m, 2H), 0.68 (m, 2H), −0.40 (m, 1H). LC/MS (m/z): 485 (M+H)+. GPR119 Human EC50: 2.1 nM.

後処理

  1. stirringThe mixture was stirred at RT overnight
  2. customThe desired product (Rf=0.35 @ pure EtOAc) was collected

出典と根拠

ORDレコード
ord-ab43a2e2c3b0445ea933ba05e1851f8d
出典データセット
uspto-grants-2015_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09018224B2

反応ノート

読み込み中…

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