Hydrochloric Acid → HCID 58259952、化合物

HRID 1020205ノート

反応式

HRID 1020205 の反応式
[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]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 441819591-(Prop-2-en-1-yl)cyclopropane-1-sulfonyl chlorideHCID 58990848HCID 58990848、化合物

生成物 1

HCID 58259952HCID 58259952、化合物

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-9636b797a1f14acca6573b2008d25429
出典データセット
uspto-grants-2014_05
特許番号
US08716318B2

反応ノート

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