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Hydrochloric Acid → HCID 178422703、化合物

HRID 1604607
ノート
印刷プレビュー

反応式

HRID 1604607 の反応式
[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
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 313Hydrochloric AcidHCID 178422702HCID 178422702、化合物

生成物 1

HCID 178422703HCID 178422703、化合物収率 31.5%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒2 回HCID 8857Ethyl Acetate溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-3d7b675bde444362a70dc2aa6ef55dd5
出典データセット
uspto-grants-1999_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05994368

反応ノート

読み込み中…

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