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Diethyl Ether → HCID 22009300, 화합물

HRID 323289
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HRID 323289 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:48]=[C:49]([O:53][CH3:54])[C:50]=1[O:51][CH3:52])[C:6]([N:8]1[CH2:12][CH2:11][C:10]([CH2:19][CH2:20][N:21]2[CH2:26][CH2:25][CH:24]([NH:27][C:28]3[N:32]([CH2:33][C:34]4[CH:39]=[CH:38][CH:37]=[CH:36][C:35]=4[C:40]([O:42]C)=[O:41])[C:31]4[CH:44]=[CH:45][CH:46]=[CH:47][C:30]=4[N:29]=3)[CH2:23][CH2:22]2)([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[CH2:9]1)=[O:7].O.[OH-].[Li+].[CH3:58][S:59]([OH:62])(=[O:61])=[O:60].C(OCC)C>O1CCCC1.O>[CH3:58][S:59]([OH:62])(=[O:61])=[O:60].[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:48]=[C:49]([O:53][CH3:54])[C:50]=1[O:51][CH3:52])[C:6]([N:8]1[CH2:12][CH2:11][C:10]([CH2:19][CH2:20][N:21]2[CH2:22][CH2:23][CH:24]([NH:27][C:28]3[N:32]([CH2:33][C:34]4[CH:39]=[CH:38][CH:37]=[CH:36][C:35]=4[C:40]([OH:42])=[O:41])[C:31]4[CH:44]=[CH:45][CH:46]=[CH:47][C:30]=4[N:29]=3)[CH2:25][CH2:26]2)([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[CH2:9]1)=[O:7]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 3283Diethyl EtherHCID 6395Methanesulfonic AcidHCID 168937Lithium hydroxide, monohydrateHCID 9896732HCID 9896732, 화합물

생성물 1

HCID 22009300HCID 22009300, 화합물

시약·촉매·용매 2

HCID 962Water용매
HCID 8028
Tetrahydrofuran
용매
2회

실험 절차

Combine 1-(3,4,5-trimethoxybenzoyl)-3-(2-(4-(1-(2-methoxycarbonylbenzyl)-1H-benzimidazol-2-yl-amino)piperidin-1-yl)ethyl)-3-phenylpyrrolidine (0.6 g, 0.8 mmol) and lithium hydroxide hydrate (0.11 g, 2.4 mmol) in tetrahydrofuran (24 mL) and water (8 mL). After 18 hours, evaporate the reaction mixture in vacuo to remove the tetrahydrofuran to obtain a solid. Collect the solid and add tetrahydrofuran (40 mL). Add a solution of methanesulfonic acid (0.24 g, 2.6 mmol) in tetrahydrofuran (3 mL). Add diethyl ether (200 mL) to give a residue. Decant the supernatant, add diethyl ether, and stir to give a solid. Collect the solid and dry in vacuo to give the title compound: mp; 161-175° C.

후처리

  1. customevaporate the reaction mixture in vacuo
  2. customto remove the tetrahydrofuran
  3. customto obtain a solid
  4. customCollect the solid
  5. additionadd tetrahydrofuran (40 mL)
  6. customDecant the supernatant
  7. additionadd diethyl ether
  8. customto give a solid
  9. customCollect the solid
  10. customdry in vacuo

출처 및 근거

ORD 기록
ord-cb92093ff0a64665953fd39aa6a36627
출처 데이터셋
uspto-grants-2001_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06211199B1

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