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Hydrochloric Acid → HCID 178422703, 화합물

HRID 1604607
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HRID 1604607 반응식
[Cl:1][C:2]1[C:20]([N:21]([C:23](=[O:54])[CH2:24][NH:25][C:26](=[O:53])[CH:27]=[CH:28][C:29]2[CH:34]=[CH:33][C:32]([NH:35][C:36]([NH:45]C(OC(C)(C)C)=O)=[N:37]C(OC(C)(C)C)=O)=[CH:31][CH:30]=2)[CH3:22])=[CH:19][CH:18]=[C:17]([Cl:55])[C:3]=1[CH2:4][O:5][C:6]1[CH:7]=[CH:8][CH:9]=[C:10]2[C:15]=1[N:14]=[C:13]([CH3:16])[CH:12]=[CH:11]2.Cl>C(OCC)(=O)C.CO>[Cl:1][C:2]1[C:20]([N:21]([C:23](=[O:54])[CH2:24][NH:25][C:26](=[O:53])[CH:27]=[CH:28][C:29]2[CH:30]=[CH:31][C:32]([NH:35][C:36]([NH2:45])=[NH:37])=[CH:33][CH:34]=2)[CH3:22])=[CH:19][CH:18]=[C:17]([Cl:55])[C:3]=1[CH2:4][O:5][C:6]1[CH:7]=[CH:8][CH:9]=[C:10]2[C:15]=1[N:14]=[C:13]([CH3:16])[CH:12]=[CH:11]2
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 313Hydrochloric AcidHCID 178422702HCID 178422702, 화합물

생성물 1

HCID 178422703HCID 178422703, 화합물수율 31.5%

시약·촉매·용매 2

HCID 887Methanol용매2회HCID 8857Ethyl Acetate용매

실험 절차

To a solution of 8-[2,6-dichloro-3-[N-[4-[2,3-bis(tert-butoxycarbonyl)guanidino]cinnamoylglycyl]-N-methylamino]benzyloxy]-2-methylquinoline (51 mg) in ethyl acetate and methanol was added 4N solution of hydrogen chloride in methanol (0.5 ml), and themixture was stirred for 2 days at ambient temperature. The mixture was concentrated in vacuo, and the residuewas dissolved in methaol. The solution was adjusted to pH 7 to 8 with aqueous ammonia and concentrated in vacuo. The residue was purified by preparative thin-layer chromatography (chloroform-methanol-aqueous ammonia) to give 8-[2,6-dichloro-3-[N-(4-guanidinocinnamoylglycyl)-N-methylamino]benzyloxy]-2-methylquinoline (12 mg) as amorphous powder.

후처리

  1. concentrationThe mixture was concentrated in vacuo
  2. dissolutionthe residuewas dissolved in methaol
  3. concentrationconcentrated in vacuo
  4. customThe residue was purified by preparative thin-layer chromatography (chloroform-methanol-aqueous ammonia)

출처 및 근거

ORD 기록
ord-3d7b675bde444362a70dc2aa6ef55dd5
출처 데이터셋
uspto-grants-1999_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05994368

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