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Sodium Thiosulfate → HCID 22938752, 화합물

HRID 856719
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HRID 856719 반응식
[H-].[Li+].[Al+3].[H-].[H-].[H-].[CH2:7]([N:10]1[CH:14]=[C:13]([C:15](OC)=[O:16])[N:12]=[N:11]1)[CH2:8][CH3:9].S([O-])([O-])(=O)=S.[Na+].[Na+]>C1COCC1>[OH:16][CH2:15][C:13]1[N:12]=[N:11][N:10]([CH2:7][CH2:8][CH3:9])[CH:14]=1
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참가 물질

5

반응물 3

HCID 24477Sodium ThiosulfateHCID 21226445Aluminium lithium hydrideHCID 22938529Methyl 1-propyl-1H-1,2,3-triazole-4-carboxylate

생성물 1

HCID 22938752HCID 22938752, 화합물수율 87.6%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

To a solution of aluminum lithium hydride (0.58 g) in THF (51.4 ml) was added dropwise a solution of methyl 1-propyl-1,2,3-triazole-4-carboxylate (2.6 g) in THF (26 ml) at 0° C. The mixture was stirred for 1 hour at room temperature, and an aqueous solution of saturated sodium thiosulfate was added to the mixture at 0° C. The mixture was filtered with Celite, and washed with ethanol. The solvent was removed under reduced pressure, and the obtained residue was purified by silica gel column chromatography, to give 4-hydroxymethyl-1-propyl-1,2,3-triazole (1.9 g). To 4-hydroxymethyl-1-propyl-1,2,3-triazole (1.9 g) was added thionyl chloride (32 ml) at 0° C., and the mixture was heated to reflux for 1 hour. After allowing the mixture to be cooled to room temperature, the solvent was removed under reduced pressure, to give 4-chloromethyl-1-propyl-1,2,3-triazole (1.75 g).

후처리

  1. filtrationThe mixture was filtered with Celite
  2. washwashed with ethanol
  3. customThe solvent was removed under reduced pressure
  4. customthe obtained residue was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-6d6f93c1d8db4bc994ec1f6a135dfcc0
출처 데이터셋
uspto-grants-2007_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07262185B2

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