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Sulfuric Acid → HCID 59136055、化合物

HRID 504950
ノート
印刷プレビュー

反応式

HRID 504950 の反応式
CO[CH:3](OC)[CH:4]1[S:8][C:7]([C:9]2[NH:10][C:11]3[C:16]([CH:17]=2)=[CH:15][C:14]([O:18][CH2:19][CH2:20][O:21][CH3:22])=[CH:13][C:12]=3[N:23]([CH3:33])[S:24]([C:27]2[N:28]([CH3:32])[CH:29]=[CH:30][N:31]=2)(=[O:26])=[O:25])=[N:6][CH2:5]1.FC(F)(F)C(O)=O.S(=O)(=O)(O)O.Cl.[NH:49]1[CH2:54][CH2:53][S:52](=[O:55])[CH2:51][CH2:50]1.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+]>O1CCCC1.O.C(N(CC)CC)C>[CH3:22][O:21][CH2:20][CH2:19][O:18][C:14]1[CH:15]=[C:16]2[C:11](=[C:12]([N:23]([CH3:33])[S:24]([C:27]3[N:28]([CH3:32])[CH:29]=[CH:30][N:31]=3)(=[O:25])=[O:26])[CH:13]=1)[NH:10][C:9]([C:7]1[S:8][CH:4]([CH2:3][N:49]3[CH2:54][CH2:53][S:52](=[O:55])[CH2:51][CH2:50]3)[CH2:5][N:6]=1)=[CH:17]2
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

9

反応物 5

HCID 1118Sulfuric AcidHCID 6422Trifluoroacetic acidHCID 5049666Sodium triacetoxyborohydrideHCID 204414791Lambda4-thiomorpholin-1-one hydrochlorideHCID 59135952HCID 59135952、化合物

生成物 1

HCID 59136055HCID 59136055、化合物収率 18%

試薬・触媒・溶媒

3
HCID 962Water溶媒2 回HCID 8028Tetrahydrofuran溶媒HCID 8471Triethylamine溶媒

反応条件

温度
60 °C

実験手順

To a mixture of N-[2-[5-(dimethoxymethyl)-4,5-dihydro-1,3-thiazol-2-yl]-5-(2-methoxyethoxy)-1H-indol-7-yl]-N,1-dimethyl-1H-imidazole-2-sulfonamide (280 mg), trifluoroacetic acid (3.5 mL) and water (10.5 mL) was added concentrated sulfuric acid (3.5 mL), and the mixture was stirred at 60° C. for 3.5 hr. The excess trifluoroacetic acid was evaporated under reduced pressure, and the residue was neutralized with sodium hydrogencarbonate. The reaction mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine, dried over magnesium sulfate, and filtrated, and the filtrate was concentrated under reduced pressure. The obtained crude product was dissolved in tetrahydrofuran (10 mL), thiomorpholine 1-oxide hydrochloride (103 mg) and triethylamine (0.1 mL) were added, and the mixture was stirred at room temperature for 15 min. Sodium triacetoxyborohydride (233 mg) was added, and the mixture was stirred at room temperature for 16 hr. Water was added to the reaction solution, and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine, dried over magnesium sulfate, and filtrated, and the filtrate was concentrated under reduced pressure. The residue was silica gel column chromatography (methanol:ethyl acetate=0:100-10:90), and the obtained crude product was further purified by preparative HPLC to give the title compound (56 mg, yield 18%) as a white solid. MS: 581 (MH+).

後処理

  1. customThe excess trifluoroacetic acid was evaporated under reduced pressure
  2. extractionThe reaction mixture was extracted with ethyl acetate
  3. washThe organic layer was washed with saturated brine
  4. dry with materialdried over magnesium sulfate
  5. filtrationfiltrated
  6. concentrationthe filtrate was concentrated under reduced pressure
  7. customThe obtained crude product
  8. stirringthe mixture was stirred at room temperature for 15 min
  9. stirringthe mixture was stirred at room temperature for 16 hr
  10. extractionthe mixture was extracted with ethyl acetate
  11. washThe organic layer was washed with saturated brine
  12. dry with materialdried over magnesium sulfate
  13. filtrationfiltrated
  14. concentrationthe filtrate was concentrated under reduced pressure
  15. customthe obtained crude product
  16. customwas further purified by preparative HPLC

出典と根拠

ORDレコード
ord-c85418fc68be4bd092a165707b2d8b9e
出典データセット
uspto-grants-2010_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07777047B2

反応ノート

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