Triethylamine → [2-(3-{3-[(2-Chloro-3-trifluoromethyl-benzyl)-diphenylethyl-amino]-propoxy}-phenyl)-ethyl]-pyrimidin-2-yl-amine hydrochloride salt

HRID 902697ノート

反応式

HRID 902697 の反応式
[NH2:1][CH2:2][CH2:3][C:4]1[CH:5]=[C:6]([CH:38]=[CH:39][CH:40]=1)[O:7][CH2:8][CH2:9][CH2:10][N:11]([CH2:26][C:27]1[CH:32]=[CH:31][CH:30]=[C:29]([C:33]([F:36])([F:35])[F:34])[C:28]=1[Cl:37])[CH2:12][CH:13]([C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1)[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1.Cl[C:42]1[N:47]=[CH:46][CH:45]=[CH:44][N:43]=1.C(N(CC)CC)C>C(O)C>[ClH:37].[Cl:37][C:28]1[C:29]([C:33]([F:34])([F:35])[F:36])=[CH:30][CH:31]=[CH:32][C:27]=1[CH2:26][N:11]([CH2:12][CH:13]([C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1)[C:14]1[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=1)[CH2:10][CH2:9][CH2:8][O:7][C:6]1[CH:5]=[C:4]([CH2:3][CH2:2][NH:1][C:42]2[N:47]=[CH:46][CH:45]=[CH:44][N:43]=2)[CH:40]=[CH:39][CH:38]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 744042-ChloropyrimidineHCID 59701396HCID 59701396、化合物

生成物 1

HCID 69252291[2-(3-{3-[(2-Chloro-3-trifluoromethyl-benzyl)-diphenylethyl-amino]-propoxy}-phenyl)-ethyl]-pyrimidin-2-yl-amine hydrochloride salt

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a stirring solution of {3-[3-(2-amino-ethyl)-phenoxy]-propyl}-(2-chloro-3-trifluoromethyl-benzyl)-(2,2-diphenyl-ethyl)-amine (57 mg, 0.1 mml, Example 150) and 2-Chloro-pyrimidine (97 mg, 0.85 mmol) in ethanol (10 mL) was added triethylamine (0.5 ml, 3.75 mmol). The resulting solution was refluxed for 72 hours and then concentrated in vacuo. Purification by preparative HPLC (YMC 75×30 mm, 25 m/min, 95-100% CH3CN) afforded the desired pyrimidine product. The free base was treated with 1 M HCl in Et2O (0.1 ml) and the mixture was concentrated in vacuo to afford the title compound as a solid, 44 mg (64%). MS(ES) m/e 645.4 (M+).

後処理

  1. temperatureThe resulting solution was refluxed for 72 hours
  2. concentrationconcentrated in vacuo
  3. customPurification by preparative HPLC (YMC 75×30 mm, 25 m/min, 95-100% CH3CN)

出典と根拠

ORDレコード
ord-19579e3047e24962b0006bdb59b13099
出典データセット
uspto-grants-2008_04
特許番号
US07365085B2

反応ノート

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