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Methanesulfonyl chloride → HCID 10472404, 화합물

HRID 1087205
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HRID 1087205 반응식
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([C:8](=[O:10])[CH3:9])=[CH:4][C:3]=1[NH:11][C:12]1[CH:17]=[CH:16][C:15]([F:18])=[CH:14][C:13]=1[F:19].[CH3:20][S:21](Cl)(=[O:23])=[O:22]>N1C=CC=CC=1>[C:8]([C:5]1[CH:6]=[CH:7][C:2]([NH:1][S:21]([CH3:20])(=[O:23])=[O:22])=[C:3]([NH:11][C:12]2[CH:17]=[CH:16][C:15]([F:18])=[CH:14][C:13]=2[F:19])[CH:4]=1)(=[O:10])[CH3:9]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 31297Methanesulfonyl chlorideHCID 10378008HCID 10378008, 화합물

생성물 1

HCID 10472404HCID 10472404, 화합물수율 58.9%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

A mixture of 4'-amino-3'-(2,4-difluorophenylamino)acetophenone (1.7 g) and methanesulfonyl chloride (0.9 g) in pyridine (17 ml) was stirred for 4 hours at room temperature. Pyridine was evaporated and the residue was stirred with an aqueous solution of sodium hydroxide (5%) for 30 minutes. The solution was washed with toluene, acidified to pH 3 with hydrochloric acid, and extracted with ethyl acetate. The extract was washed with an aqueous solution of sodium bicarbonate, dried, and concentrated under reduced pressure. The syrupy residue (1.8 g) was crystallized from ethanol to give pale yellow crystals of 4'-acetyl-2'-(2,4-difluorophenylamino)methanesulfonanilide (1.3 g).

후처리

  1. customPyridine was evaporated
  2. stirringthe residue was stirred with an aqueous solution of sodium hydroxide (5%) for 30 minutes
  3. washThe solution was washed with toluene
  4. extractionextracted with ethyl acetate
  5. washThe extract was washed with an aqueous solution of sodium bicarbonate
  6. customdried
  7. concentrationconcentrated under reduced pressure
  8. customThe syrupy residue (1.8 g) was crystallized from ethanol

출처 및 근거

ORD 기록
ord-d9434fbdde084013836e46ee42d0a47a
출처 데이터셋
uspto-grants-1991_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05034417

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