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4-Methylpiperazine-1-ethylamine → N4-(5-Isopropyl-1H-pyrazol-3-yl)-N6-[2-(4-methylpiperazin-1-yl)ethyl]-N2-(3-phenylisoxazol-5-ylmethyl)-pyrimidine-2,4,6-triamine

HRID 1514325
ノート
印刷プレビュー

反応式

HRID 1514325 の反応式
Cl[C:2]1[N:7]=[C:6]([NH:8][CH2:9][C:10]2[O:14][N:13]=[C:12]([C:15]3[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=3)[CH:11]=2)[N:5]=[C:4]([NH:21][C:22]2[CH:26]=[C:25]([CH:27]([CH3:29])[CH3:28])[NH:24][N:23]=2)[CH:3]=1.[CH3:30][N:31]1[CH2:36][CH2:35][N:34]([CH2:37][CH2:38][NH2:39])[CH2:33][CH2:32]1>C(O)CCC.CO>[CH:27]([C:25]1[NH:24][N:23]=[C:22]([NH:21][C:4]2[CH:3]=[C:2]([NH:39][CH2:38][CH2:37][N:34]3[CH2:35][CH2:36][N:31]([CH3:30])[CH2:32][CH2:33]3)[N:7]=[C:6]([NH:8][CH2:9][C:10]3[O:14][N:13]=[C:12]([C:15]4[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=4)[CH:11]=3)[N:5]=2)[CH:26]=1)([CH3:29])[CH3:28]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 702844-Methylpiperazine-1-ethylamineHCID 578664486-Chloro-N4-(5-isopropyl-1H-pyrazol-3-yl)-N2-(3-phenylisoxazol-5-ylmethyl)-pyrimidine-2,4-diamine

生成物 1

HCID 59757794N4-(5-Isopropyl-1H-pyrazol-3-yl)-N6-[2-(4-methylpiperazin-1-yl)ethyl]-N2-(3-phenylisoxazol-5-ylmethyl)-pyrimidine-2,4,6-triamine収率 29.5%

試薬・触媒・溶媒 2

HCID 2631-Butanol溶媒
HCID 887
Methanol
溶媒

反応条件

温度
180 °C

実験手順

A mixture of 6-chloro-N4-(5-isopropyl-1H-pyrazol-3-yl)-N2-(3-phenylisoxazol-5-ylmethyl)-pyrimidine-2,4-diamine (250 mg, 0.611 mmol) and 2-(4-methylpiperazin-1-yl)-ethylamine (500 mg, 3.50 mmol) in 1-butanol (2 mL) was heated to 180° C. in a 50 mL sealed tube. The mixture was heated for 1 h, then cooled to room temperature and diluted with methanol (10 mL). The mixture thus obtained was purified via preparative reverse phase HPLC to give the desired product (93 mg, 29%) as a white solid.

後処理

  1. customsealed tube
  2. temperatureThe mixture was heated for 1 h
  3. temperaturecooled to room temperature
  4. customThe mixture thus obtained
  5. customwas purified via preparative reverse phase HPLC

出典と根拠

ORDレコード
ord-5d1d83e5a66c4d78b3d7b819f152a778
出典データセット
uspto-grants-2012_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08222256B2

反応ノート

読み込み中…

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