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Succinic Acid → n-{5-[(1r)-2-({2-[4-(2-{3-[(1r)-3-(Diisopropylamino)-1-phenylpropyl]-4-hydroxyphenyl}ethoxy)phenyl]ethyl}amino)-1-hydroxyethyl]-2-hydroxyphenyl}methanesulfonamide succinate salt

HRID 1433308
ノート
印刷プレビュー

反応式

HRID 1433308 の反応式
[CH:1]([N:4]([CH:48]([CH3:50])[CH3:49])[CH2:5][CH2:6][C@@H:7]([C:14]1[CH:15]=[C:16]([CH2:21][CH2:22][O:23][C:24]2[CH:29]=[CH:28][C:27]([CH2:30][CH2:31][NH:32][CH2:33][C@@H:34]([C:36]3[CH:37]=[CH:38][C:39]([OH:47])=[C:40]([NH:42][S:43]([CH3:46])(=[O:45])=[O:44])[CH:41]=3)[OH:35])=[CH:26][CH:25]=2)[CH:17]=[CH:18][C:19]=1[OH:20])[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)([CH3:3])[CH3:2].[C:51]([OH:58])(=[O:57])[CH2:52][CH2:53][C:54]([OH:56])=[O:55]>CO.O>[C:51]([OH:58])(=[O:57])[CH2:52][CH2:53][C:54]([OH:56])=[O:55].[CH:48]([N:4]([CH:1]([CH3:3])[CH3:2])[CH2:5][CH2:6][C@@H:7]([C:14]1[CH:15]=[C:16]([CH2:21][CH2:22][O:23][C:24]2[CH:29]=[CH:28][C:27]([CH2:30][CH2:31][NH:32][CH2:33][C@@H:34]([C:36]3[CH:37]=[CH:38][C:39]([OH:47])=[C:40]([NH:42][S:43]([CH3:46])(=[O:45])=[O:44])[CH:41]=3)[OH:35])=[CH:26][CH:25]=2)[CH:17]=[CH:18][C:19]=1[OH:20])[C:8]1[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=1)([CH3:50])[CH3:49]
参加物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 1110Succinic AcidHCID 57933169N-{5-[(1R)-2-({2-[4-(2-{3-[(1R)-3-(diisopropylamino)-1-phenylpropyl]-4-hydroxyphenyl}ethoxy)phenyl]ethyl}amino)-1-hydroxyethyl]-2-hydroxyphenyl}methanesulfonamide

生成物 1

HCID 68928990n-{5-[(1r)-2-({2-[4-(2-{3-[(1r)-3-(Diisopropylamino)-1-phenylpropyl]-4-hydroxyphenyl}ethoxy)phenyl]ethyl}amino)-1-hydroxyethyl]-2-hydroxyphenyl}methanesulfonamide succinate salt

試薬・触媒・溶媒 2

HCID 887
Methanol
溶媒
2 回
HCID 962Water溶媒2 回

実験手順

N-{5-[(1R)-2-({2-[4-(2-{3-[(1R)-3-(diisopropylamino)-1-phenylpropyl]-4-hydroxyphenyl}ethoxy)phenyl]ethyl}amino)-1-hydroxyethyl]-2-hydroxyphenyl}methanesulfonamide (Example 5, 2000 mg, 2.84 mmol) was dissolved in methanol (8 ml) and succinic acid (336 mg, 2.84 mmol) in water (2 ml) and methanol (2 ml) was added in one portion to the stirred solution at room temperature. Further water was added until the salt appeared as a gum which was seeded with a small crystal of the salt previously isolated. The mixture was left overnight and stirred occasionally to aid crystallisation. After 5 days the solid was filtered and dried in vacuo to furnish the title compound as a white crystalline solid, 2336 mg, m.p. 148-150° C.

後処理

  1. custompreviously isolated
  2. customcrystallisation
  3. filtrationAfter 5 days the solid was filtered
  4. customdried in vacuo

出典と根拠

ORDレコード
ord-65ec2149093841d7b2d5e3bf1bcd7952
出典データセット
uspto-grants-2009_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07612084B2

反応ノート

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