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

HRID 413821

반응식

HRID 413821 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 min. and at room temperature for 3 hr. The resulting dark colored reaction mixture was carefully poured into an ice-water mixture (200 mL) and stirred at room temperature for 30 min. The resulting precipitate was filtered and washed thoroughly with cold water (500 ml). The solid was dried overnight under high vacuum in a desiccator over NaOH pallets to yield the desired compound (5.9 g. 78%) as a grey powder. 1H NMR (DMSO-d6) 3.89 (s, 3H), 7.55 (d, 1H, J=8.4 Hz.) 7.65 (d, 1H, J=8.4 Hz), 7.88 (s, 1H).

후처리

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

출처 및 근거

ORD 기록
ord-bc7c9f9a35404be49ec29414babf70be
출처 데이터셋
uspto-grants-2003_05
특허 번호
US06569882B2

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