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

HRID 1727104
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HRID 1727104 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 6395Methanesulfonic AcidHCID 12986481UP9V9DB2RD

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-5dc419a3ae4b4cd88ac5cdc37ac19b4c
출처 데이터셋
uspto-grants-2009_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07494987B2

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