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1H-Imidazole-2-methanol, 5-((3,5-dichlorophenyl)thio)-4-(1-methylethyl)-1-((3-nitrophenyl)methyl)- → 1H-Imidazole-2-methanol, 1-((3-aminophenyl)methyl)-5-((3,5-dichlorophenyl)thio)-4-(1-methylethyl)-

HRID 1416044
ノート
印刷プレビュー

反応式

HRID 1416044 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([S:9][C:10]2[N:14]([CH2:15][C:16]3[CH:21]=[CH:20][CH:19]=[C:18]([N+:22]([O-])=O)[CH:17]=3)[C:13]([CH2:25][OH:26])=[N:12][C:11]=2[CH:27]([CH3:29])[CH3:28])[CH:5]=[C:6]([Cl:8])[CH:7]=1.[H][H]>C(OCC)(=O)C.[Pt]>[NH2:22][C:18]1[CH:17]=[C:16]([CH:21]=[CH:20][CH:19]=1)[CH2:15][N:14]1[C:10]([S:9][C:4]2[CH:5]=[C:6]([Cl:8])[CH:7]=[C:2]([Cl:1])[CH:3]=2)=[C:11]([CH:27]([CH3:29])[CH3:28])[N:12]=[C:13]1[CH2:25][OH:26]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 4740321H-Imidazole-2-methanol, 5-((3,5-dichlorophenyl)thio)-4-(1-methylethyl)-1-((3-nitrophenyl)methyl)-HCID 178418361HCID 178418361、化合物

生成物 1

HCID 4740331H-Imidazole-2-methanol, 1-((3-aminophenyl)methyl)-5-((3,5-dichlorophenyl)thio)-4-(1-methylethyl)-

試薬・触媒・溶媒 2

HCID 23939Platinum触媒HCID 8857Ethyl Acetate溶媒

実験手順

In ethyl acetate was dissolved 64 mg of 5-(3,5-dichlorophenylthio)-2-hydroxymethyl-4-isopropyl-1-(m-nitrobenzyl)-1H-imidazole (103b), and platinum sulfided carbon was added. After replacement with hydrogen atomosphere, the mixture was catalytically hydrogenated under atmospheric pressure at room temperature. After 3 hours, the mixture was filtered through Celite, the filtrate was distilled off under reduced pressure, and diethyl ether was added. Crystals precipitated were filtered, and 25 mg of Compound I-118 was obtained (yield 42%). mp 145-148° C.

後処理

  1. additionwas added
  2. customwas catalytically hydrogenated under atmospheric pressure at room temperature
  3. filtrationthe mixture was filtered through Celite
  4. distillationthe filtrate was distilled off under reduced pressure, and diethyl ether
  5. additionwas added
  6. customCrystals precipitated
  7. filtrationwere filtered
  8. customwas obtained (yield 42%)

出典と根拠

ORDレコード
ord-9bc3056dc16a46518d2321d0f0867119
出典データセット
uspto-grants-1999_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05910506

反応ノート

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