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Methanesulfonic Acid → 4-[(4-Methylpiperazin-1-yl)methyl]-n-{6-methyl-5-[(4-(pyrid-3-yl)pyrimid-2-yl)amino]pyrid-3-yl} benzamide methanesulfonic acid salt

HRID 1926594
ノート
印刷プレビュー

反応式

HRID 1926594 の反応式
[CH3:1][N:2]1[CH2:7][CH2:6][N:5]([CH2:8][C:9]2[CH:37]=[CH:36][C:12]([C:13]([NH:15][C:16]3[CH:17]=[N:18][C:19]([CH3:35])=[C:20]([NH:22][C:23]4[N:28]=[C:27]([C:29]5[CH:30]=[N:31][CH:32]=[CH:33][CH:34]=5)[CH:26]=[CH:25][N:24]=4)[CH:21]=3)=[O:14])=[CH:11][CH:10]=2)[CH2:4][CH2:3]1.[CH3:38][S:39]([OH:42])(=[O:41])=[O:40]>CO>[CH3:38][S:39]([OH:42])(=[O:41])=[O:40].[CH3:1][N:2]1[CH2:7][CH2:6][N:5]([CH2:8][C:9]2[CH:10]=[CH:11][C:12]([C:13]([NH:15][C:16]3[CH:17]=[N:18][C:19]([CH3:35])=[C:20]([NH:22][C:23]4[N:28]=[C:27]([C:29]5[CH:30]=[N:31][CH:32]=[CH:33][CH:34]=5)[CH:26]=[CH:25][N:24]=4)[CH:21]=3)=[O:14])=[CH:36][CH:37]=2)[CH2:4][CH2:3]1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 6395Methanesulfonic AcidHCID 692278004-[(4-methylpiperazin-1-yl)methyl]-N-{6-methyl-5-[(4-(pyrid-3-yl)pyrimid-2-yl)amino]pyrid-3-yl}benzamide

生成物 1

HCID 877440834-[(4-Methylpiperazin-1-yl)methyl]-n-{6-methyl-5-[(4-(pyrid-3-yl)pyrimid-2-yl)amino]pyrid-3-yl} benzamide methanesulfonic acid salt収率 83.7%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a flask was added 4-[(4-methylpiperazin-1-yl)methyl]-N-{6-methyl-5-[(4-(3-pyridyl)-2-pyrimidyl)amino]-3-pyridyl}benzamide (2.0 g), methanesulfonic acid (0.40 g) and methanol (100 mL). After the solution was clear, the reaction mixture was concentrated under reduced pressure to about 20 mL and acetone was added to get a crystal. Filtrated and the solid was dried to give 4-[(4-methylpiperazin-1-yl)methyl]-N-{6-methyl-5-[(4-(pyrid-3-yl)pyrimid-2-yl)amino]pyrid-3-yl} benzamide methanesulfonic acid salt (2.0 g).

後処理

  1. concentrationthe reaction mixture was concentrated under reduced pressure to about 20 mL and acetone
  2. additionwas added
  3. customto get a crystal
  4. filtrationFiltrated
  5. customthe solid was dried

出典と根拠

ORDレコード
ord-ced7181a8b6a43d3a80d7bd66728e2db
出典データセット
uspto-grants-2012_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08183242B2

反応ノート

読み込み中…

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