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Methanesulfonic Acid → 4-({1-[2-(4-Cyanophenyl)ethyl]-4-hydroxypiperidin-4-ylmethyl}methylamino)benzoic acid monomethanesulfonate

HRID 1727104
ノート
印刷プレビュー

反応式

HRID 1727104 の反応式
[CH3:1][S:2]([OH:5])(=[O:4])=[O:3].[C:6]([C:8]1[CH:13]=[CH:12][C:11]([CH2:14][CH2:15][N:16]2[CH2:21][CH2:20][C:19]([CH2:23][N:24]([CH3:34])[C:25]3[CH:33]=[CH:32][C:28]([C:29]([OH:31])=[O:30])=[CH:27][CH:26]=3)([OH:22])[CH2:18][CH2:17]2)=[CH:10][CH:9]=1)#[N:7]>O>[CH3:1][S:2]([OH:5])(=[O:4])=[O:3].[C:6]([C:8]1[CH:9]=[CH:10][C:11]([CH2:14][CH2:15][N:16]2[CH2:17][CH2:18][C:19]([CH2:23][N:24]([CH3:34])[C:25]3[CH:26]=[CH:27][C:28]([C:29]([OH:31])=[O:30])=[CH:32][CH:33]=3)([OH:22])[CH2:20][CH2:21]2)=[CH:12][CH:13]=1)#[N:7]
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 12986481UP9V9DB2RD

生成物 1

HCID 866033484-({1-[2-(4-Cyanophenyl)ethyl]-4-hydroxypiperidin-4-ylmethyl}methylamino)benzoic acid monomethanesulfonate

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Methanesulfonic acid (1.42 mL) was added to a suspension of the compound (7.2 g) obtained in Example 1 in water (50 mL), was heated with stirring until the compound was dissolved, followed by cooling to room temperature with stirring. The crystals were collected by filtration and were recrystallized from water (50 mL). The resulting crystals were collected by filtration, washed with acetone, and dried under reduced pressure to yield the titled compound (7.6 g) as crystals.

後処理

  1. temperaturewas heated
  2. dissolutionwas dissolved
  3. stirringwith stirring
  4. filtrationThe crystals were collected by filtration
  5. customwere recrystallized from water (50 mL)
  6. filtrationThe resulting crystals were collected by filtration
  7. washwashed with acetone
  8. customdried under reduced pressure

出典と根拠

ORDレコード
ord-5dc419a3ae4b4cd88ac5cdc37ac19b4c
出典データセット
uspto-grants-2009_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07494987B2

反応ノート

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