Diisopropylethylamine → 5-Methyl-2-{4-[(2-methyl-pyrimidin-5-ylmethyl)-amino]-7,8-dihydro-5H-pyrido[4,3-d]pyrimidin-6-yl}-benzonitrile

HRID 657800

反応式

HRID 657800 の反応式
Cl[C:2]1[C:3]2[CH2:11][N:10]([C:12]3[CH:19]=[CH:18][C:17]([CH3:20])=[CH:16][C:13]=3[C:14]#[N:15])[CH2:9][CH2:8][C:4]=2[N:5]=[CH:6][N:7]=1.[CH3:21][C:22]1[N:27]=[CH:26][C:25]([CH2:28][NH2:29])=[CH:24][N:23]=1.C(N(CC)C(C)C)(C)C>C(#N)C>[CH3:20][C:17]1[CH:18]=[CH:19][C:12]([N:10]2[CH2:9][CH2:8][C:4]3[N:5]=[CH:6][N:7]=[C:2]([NH:29][CH2:28][C:25]4[CH:24]=[N:23][C:22]([CH3:21])=[N:27][CH:26]=4)[C:3]=3[CH2:11]2)=[C:13]([CH:16]=1)[C:14]#[N:15]

参加物

5

反応物 3

HCID 81531DiisopropylethylamineHCID 21294601(2-Methylpyrimidin-5-yl)methanamineHCID 598406882-(4-Chloro-7,8-dihydropyrido[4,3-d]pyrimidin-6(5H)-yl)-5-methylbenzonitrile

生成物 1

HCID 250592895-Methyl-2-{4-[(2-methyl-pyrimidin-5-ylmethyl)-amino]-7,8-dihydro-5H-pyrido[4,3-d]pyrimidin-6-yl}-benzonitrile

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

A reaction mixture of 2-(4-chloro-7,8-dihydropyrido[4,3-d]pyrimidin-6(5H)-yl)-5-methylbenzonitrile (400 mg, 1.41 mmol) and (2-methylpyrimidin-5-yl)methanamine (400 mg, 3.25 mmol) in acetonitrile (3 mL) and N,N-diisopropylethylamine (1.5 mL, 8.6 mmol) was subjected to microwave irradiation at 185° C. for 2.5 h. The reaction mixture was concentrated and purified by preparative HPLC (100×20.2 mm, C18 column; 40-60% CH3CN-water [10 mM Et2NH]) to yield a light brown solid.

後処理

  1. customirradiation at 185° C. for 2.5 h
  2. concentrationThe reaction mixture was concentrated
  3. custompurified by preparative HPLC (100×20.2 mm, C18 column; 40-60% CH3CN-water [10 mM Et2NH])
  4. customto yield a light brown solid

出典と根拠

ORDレコード
ord-a5ac386a0c3f4ffbbb0a600279d240ec
出典データセット
uspto-grants-2011_12
特許番号
US08076345B2

関連ノート

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