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

HRID 487845

반응식

HRID 487845 반응식
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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-21d61f07ab5e409ea3eec212aa4b057a
출처 데이터셋
uspto-grants-1994_03
특허 번호
US05298390

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