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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
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인쇄 미리보기

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HRID 1433308 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 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

생성물 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

시약·촉매·용매 2

HCID 887
Methanol
용매
2회
HCID 962Water용매2회

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-65ec2149093841d7b2d5e3bf1bcd7952
출처 데이터셋
uspto-grants-2009_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07612084B2

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