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Sodium Thiosulfate → HCID 22938752、化合物

HRID 856719
ノート
印刷プレビュー

反応式

HRID 856719 の反応式
[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
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 3

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

生成物 1

HCID 22938752HCID 22938752、化合物収率 87.6%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-6d6f93c1d8db4bc994ec1f6a135dfcc0
出典データセット
uspto-grants-2007_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07262185B2

反応ノート

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