Water → 1-{[(1H-1,2,3-benzotriazol-1-ylmethyl)sulfanyl]methyl}-1H-1,2,3-benzotriazole

HRID 487845

反応式

HRID 487845 の反応式
Cl[CH2:2][N:3]1[C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=2[N:5]=[N:4]1.O.[S-2:13].[Na+].[Na+].O>C(O)C>[N:3]1([CH2:2][S:13][CH2:2][N:3]2[C:7]3[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=3[N:5]=[N:4]2)[C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=2[N:5]=[N:4]1

参加物

5

反応物 3

HCID 962WaterHCID 33282221-(Chloromethyl)-1H-benzotriazoleHCID 19906495Sodium sulfide monohydrate

生成物 1

HCID 37660921-{[(1H-1,2,3-benzotriazol-1-ylmethyl)sulfanyl]methyl}-1H-1,2,3-benzotriazole収率 88%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

1-(Chloromethyl)benzotriazole (20.4 g), prepared above, and sodium sulfide monohydrate (14.4 g) in anhydrous ethanol (75 ml) were stirred overnight (20 hours) at room temperature. Water (240 ml) was added to the reaction mixture. The precipitate was filtered, washed with water to remove inorganic salts and dried. Crystallization from ethanol gave 15.6 g (88%) of desired product (Compound 1); m.p. 179°-181° C. (lit. 182°-184° C.). Thin Layer Chromotography in (CHCl3 /Ethyl acetate) showed only one spot.

後処理

  1. filtrationThe precipitate was filtered
  2. washwashed with water
  3. customto remove inorganic salts
  4. customdried
  5. customCrystallization from ethanol

出典と根拠

ORDレコード
ord-21d61f07ab5e409ea3eec212aa4b057a
出典データセット
uspto-grants-1994_03
特許番号
US05298390

関連ノート

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