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Cyanogen Bromide → 6-(Methanesulfonyl)-1H-benzimidazol-2-amine

HRID 1447178
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HRID 1447178 반응식
[CH3:1][S:2]([C:5]1[CH:10]=[CH:9][C:8]([NH2:11])=[C:7]([NH2:12])[CH:6]=1)(=[O:4])=[O:3].[N:13]#[C:14]Br>O>[NH2:13][C:14]1[NH:12][C:7]2[CH:6]=[C:5]([S:2]([CH3:1])(=[O:3])=[O:4])[CH:10]=[CH:9][C:8]=2[N:11]=1
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참가 물질

4

반응물 2

HCID 10476Cyanogen BromideHCID 69514184-(methylsulfonyl)benzene-1,2-diamine

생성물 1

HCID 128379916-(Methanesulfonyl)-1H-benzimidazol-2-amine

시약·촉매·용매 1

HCID 962Water용매

실험 절차

One mole, 186.1 g., of 4-methylsulfonyl-o-phenylenediamine was suspended in 1.2 l. of water with stirring. One mole, 106 g., of cyanogenbromide was added portionwise to the reaction mixture. The reaction mixture was stirred for 4 hours and then filtered. Sodium hydroxide, 39 g. (1 m.) in 500 ml. of water, was added to the filtrate. The aqueous mixture was cooled in an ice bath and the product crystallized. The product was collected and dried before crystallization from ethanol-ether; yield 200 g., m.p. 233°-238° C.

후처리

  1. filtrationfiltered
  2. additionof water, was added to the filtrate
  3. temperatureThe aqueous mixture was cooled in an ice bath
  4. customthe product crystallized
  5. customThe product was collected
  6. dry with materialdried before crystallization from ethanol-ether

출처 및 근거

ORD 기록
ord-cc3da3ae9030418baaff05d387908f66
출처 데이터셋
uspto-grants-1982_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04316021

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