Hydrochloric Acid → HCID 58259952, 화합물

HRID 1020205노트

반응식

HRID 1020205 반응식
[NH2:1][C:2]1[C:3]([NH:10][C:11]2[CH:16]=[CH:15][C:14]([I:17])=[CH:13][C:12]=2[F:18])=[CH:4][C:5](=[O:9])[N:6]([CH3:8])[CH:7]=1.[CH2:19]([C:22]1([S:25](Cl)(=[O:27])=[O:26])[CH2:24][CH2:23]1)[CH:20]=[CH2:21].Cl>N1C=CC=CC=1>[CH2:19]([C:22]1([S:25]([NH:1][C:2]2[C:3]([NH:10][C:11]3[CH:16]=[CH:15][C:14]([I:17])=[CH:13][C:12]=3[F:18])=[CH:4][C:5](=[O:9])[N:6]([CH3:8])[CH:7]=2)(=[O:27])=[O:26])[CH2:24][CH2:23]1)[CH:20]=[CH2:21]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 441819591-(Prop-2-en-1-yl)cyclopropane-1-sulfonyl chlorideHCID 58990848HCID 58990848, 화합물

생성물 1

HCID 58259952HCID 58259952, 화합물

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

5-Amino-4-(2-fluoro-4-iodophenylamino)-1-methylpyridin-2(1H)-one (prepared as described in steps a-e in example 1 above) was dissolved in dry pyridine at 0° C. under an ice-salt bath, and 1-allylcyclopropane-1-sulfonyl chloride was added. The resultant reaction mixture was allowed to warm to room temperature. After stirring for 16 hours at room temperature, aqueous HCl (1N) was added and the mixture was stirred for 15 minutes. The formed precipitate was filtered and dried under vacuum, and purified by preparative TLC (SiO2, EtOAc:MeOH=9:1 (v:v), Rf˜0.4).

후처리

  1. customThe resultant reaction mixture
  2. stirringthe mixture was stirred for 15 minutes
  3. filtrationThe formed precipitate was filtered
  4. customdried under vacuum
  5. custompurified by preparative TLC (SiO2, EtOAc:MeOH=9:1 (v:v), Rf˜0.4)

출처 및 근거

ORD 기록
ord-9636b797a1f14acca6573b2008d25429
출처 데이터셋
uspto-grants-2014_05
특허 번호
US08716318B2

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