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Hydrochloric Acid → HCID 22176325、化合物

HRID 1797649
ノート
印刷プレビュー

反応式

HRID 1797649 の反応式
C([O:5][C:6](=[O:32])[NH:7][CH2:8][C:9]1[N:10]([CH2:28][CH:29]([CH3:31])[CH3:30])[C:11](=[O:27])[C:12]2[C:17]([C:18]=1[O:19][CH2:20][CH2:21][CH2:22][CH3:23])=[CH:16][C:15]([C:24]([NH2:26])=[S:25])=[CH:14][CH:13]=2)(C)(C)C.Cl.C(N(CC)CC)C.[CH:41]1[C:53]2[CH:52]([CH2:54]OC(Cl)=O)[C:51]3[C:46](=[CH:47][CH:48]=[CH:49][CH:50]=3)[C:45]=2[CH:44]=[CH:43][CH:42]=1>C(OCC)(=O)C.O>[NH2:26][C:24]([C:15]1[CH:16]=[C:17]2[C:12](=[CH:13][CH:14]=1)[C:11](=[O:27])[N:10]([CH2:28][CH:29]([CH3:31])[CH3:30])[C:9]([CH2:8][NH:7][C:6](=[O:32])[O:5][CH2:54][CH:52]1[C:53]3[CH:41]=[CH:42][CH:43]=[CH:44][C:45]=3[C:46]3[C:51]1=[CH:50][CH:49]=[CH:48][CH:47]=3)=[C:18]2[O:19][CH2:20][CH2:21][CH2:22][CH3:23])=[S:25]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 343679-Fluorenylmethyl chloroformateHCID 86592074HCID 86592074、化合物

生成物 1

HCID 22176325HCID 22176325、化合物収率 86.9%

試薬・触媒・溶媒 2

HCID 962Water溶媒
HCID 8857
Ethyl Acetate
溶媒

実験手順

Tert-butyl[6-(aminothiocarbonyl)-4-butoxy-2-isobutyl-1-oxo-1,2-dihydro-3-isoquinolinyl]methylcarbamate (Example 189 (1)) (1.38 g, 3 mmol) was dissolved in a solution of 4N hydrogen chloride in ethyl acetate (10 ml) and the mixture was stirred at room temperature for 1 h. The reaction mixture was concentrated under reduced pressure and the residue was suspended in tetrahydrofuran (20 ml). To the obtained mixture were added triethylamine (0.84 ml, 6 mmol) and 9-fluorenylmethylchloroformate (1.16 g, 4.5 mmol) and the mixture was stirred at 0° C. for 1 h. The reaction mixture was poured into water and extracted with ethyl acetate. The extract was washed with brine, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was purified by silica gel column chromatography to give 9H-fluoren-9-ylmethyl [6-(aminocarbothioyl)-4-butoxy-2-isobutyl-1-oxo-1,2-dihydro-3-isoquinolinyl]methylcarbamate (1.52 g, 86.9%) as an amorphous.

後処理

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. stirringthe mixture was stirred at 0° C. for 1 h
  3. extractionextracted with ethyl acetate
  4. washThe extract was washed with brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. concentrationconcentrated under reduced pressure
  7. customThe residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-6009de470d284745aba4c504fd15e74a
出典データセット
uspto-grants-2006_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07034039B2

反応ノート

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