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Dimethylformamide → 4-[4-(3-Indolyl)piperidinomethyl]-2-mesylaminothiazole

HRID 1252072
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HRID 1252072 반응식
[NH2:1][C:2]1[S:3][CH:4]=[C:5]([CH2:7][N:8]2[CH2:13][CH2:12][CH:11]([C:14]3[C:22]4[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=4)[NH:16][CH:15]=3)[CH2:10][CH2:9]2)[N:6]=1.C(N(CC)CC)C.CN(C)C=O.[S:35](Cl)([CH3:38])(=[O:37])=[O:36]>C(Cl)Cl.O>[NH:16]1[C:17]2[C:22](=[CH:21][CH:20]=[CH:19][CH:18]=2)[C:14]([CH:11]2[CH2:12][CH2:13][N:8]([CH2:7][C:5]3[N:6]=[C:2]([NH:1][S:35]([CH3:38])(=[O:37])=[O:36])[S:3][CH:4]=3)[CH2:9][CH2:10]2)=[CH:15]1
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참가 물질

7

반응물 4

HCID 6228DimethylformamideHCID 8471TriethylamineHCID 31297Methanesulfonyl chloride2회HCID 141297964-((4-(1H-Indol-3-yl)piperidin-1-yl)methyl)thiazol-2-amine

생성물 1

HCID 98005844-[4-(3-Indolyl)piperidinomethyl]-2-mesylaminothiazole

시약·촉매·용매 2

HCID 962
Water
용매
HCID 6344Dichloromethane용매2회

실험 절차

To a mixture of 2-amino-4-[4-(3-indolyl)piperidinomethyl]thiazole (1.73 g), triethylamine (3.1 ml) and N,N-dimethylformamide (15 ml) was added dropwise a solution of mesyl chloride (0.86 ml) in methylene chloride (1 ml) at 5° to 7° C. with stirring. The mixture was further stirred at that temperature for 2 hours, after which a solution of mesyl chloride (0.34 ml) in methylene chloride (0.5 ml) was added. The reaction mixture was further stirred at the same temperature for 1.5 hours. Following addition of water (50 ml), the reaction mixture was extracted with a mixture of chloroform and methanol (60 ml, 10:1 V/V) twice. The extract was washed with a saturated aqueous solution of sodium chloride, dried over magnesium sulfate, and concentrated under reduced pressure. The residue was dissolved in tetrahydrofuran (40 ml) and, then, 10% aqueous sodium hydroxide solution (20 ml) was added gradually thereto. The mixture was stirred at ambient temperature overnight. The reaction mixture was then adjusted to pH 7.0 with diluted hydrochloric acid and extracted with a mixture of chloroform and methanol (100 ml, 10:1 V/V). The organic layer was separated, washed with water, and dried over magnesium sulfate. The solvent was distilled off under reduced pressure and the residue was subjected to column chromatography on silica gel, followed by elution with a mixture of chloroform and methanol (10:1 V/V). The eluate gave 4-[4-(3-indolyl)piperidinomethyl]-2-mesylaminothiazole (480 mg).

후처리

  1. stirringThe mixture was further stirred at that temperature for 2 hours
  2. stirringThe reaction mixture was further stirred at the same temperature for 1.5 hours
  3. extractionthe reaction mixture was extracted with a mixture of chloroform and methanol (60 ml, 10:1 V/V) twice
  4. washThe extract was washed with a saturated aqueous solution of sodium chloride
  5. dry with materialdried over magnesium sulfate
  6. concentrationconcentrated under reduced pressure
  7. dissolutionThe residue was dissolved in tetrahydrofuran (40 ml)
  8. addition10% aqueous sodium hydroxide solution (20 ml) was added gradually
  9. stirringThe mixture was stirred at ambient temperature overnight
  10. extractionextracted with a mixture of chloroform and methanol (100 ml, 10:1 V/V)
  11. customThe organic layer was separated
  12. washwashed with water
  13. dry with materialdried over magnesium sulfate
  14. distillationThe solvent was distilled off under reduced pressure
  15. washfollowed by elution with a mixture of chloroform and methanol (10:1 V/V)

출처 및 근거

ORD 기록
ord-75a0dc787c494a05a58a7266cd1c18a2
출처 데이터셋
uspto-grants-1988_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04742057

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