Chlorosulfonic acid → Methyl N-[6-(chlorosulfonyl)-1H-benzimidazol-2-yl]carbamate

HRID 370338

반응식

HRID 370338 반응식
[C:1]([NH:5][C:6]1[NH:7][C:8]2[CH:14]=[CH:13][CH:12]=[CH:11][C:9]=2[N:10]=1)([O:3][CH3:4])=[O:2].[Cl:15][S:16](O)(=[O:18])=[O:17]>>[Cl:15][S:16]([C:13]1[CH:12]=[CH:11][C:9]2[N:10]=[C:6]([NH:5][C:1]([O:3][CH3:4])=[O:2])[NH:7][C:8]=2[CH:14]=1)(=[O:18])=[O:17]

참가 물질

3

반응물 2

HCID 24638Chlorosulfonic acidHCID 25429Carbendazim

생성물 1

HCID 15124047Methyl N-[6-(chlorosulfonyl)-1H-benzimidazol-2-yl]carbamate수율 78%

실험 절차

A solution of 2-carbomethoxyamino-benzimidazole (5.0 g, 0.026 mole) in chlorosulfonic acid (35.00 mL) was stirred at 0° C. for 30 minutes and at room temperature for 3 hours. The resulting dark colored reaction mixture was poured into an ice-water mixture (200 mL), and stirred at room temperature for 30 minutes. The resulting precipitate was filtered and washed with cold water (500 mL). The solid was dried overnight under high vacuum in a desiccator over NaOH pellets to give 5-chlorosulfonyl-2-carbomethoxyamino-benzimidazole (5.9 g, 78%) as a gray powder. 1H NMR (DMSO-d6) d: 3.89 (s, 3H), 7.55 (d, J=8.4 Hz, 1H), 7.65 (d, J=8.4 Hz, 1H), 7.88 (s, 1H). (German Patent DE 3826036)

후처리

  1. filtrationThe resulting precipitate was filtered
  2. washwashed with cold water (500 mL)
  3. dry with materialThe solid was dried overnight under high vacuum in a desiccator over NaOH pellets

출처 및 근거

ORD 기록
ord-feae11378b864863b9af3c7e9826592d
출처 데이터셋
uspto-grants-2000_10
특허 번호
US06140505

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