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llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
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Hexane → HCID 178502003、化合物

HRID 464770
ノート
印刷プレビュー

反応式

HRID 464770 の反応式
ClC1C=CC=C(C(OO)=[O:9])C=1.[NH2:12][C:13]1[N:18]=[C:17]([NH:19][C:20]([O:22][CH3:23])=[O:21])[CH:16]=[C:15]([O:24][S:25]([C:28]2[CH:33]=[CH:32][C:31]([CH3:34])=[CH:30][CH:29]=2)(=[O:27])=[O:26])[N:14]=1.CCCCCC>C(Cl)Cl.CO>[NH2:12][C:13]1[N+:18]([O-:9])=[C:17]([NH:19][C:20]([O:22][CH3:23])=[O:21])[CH:16]=[C:15]([O:24][S:25]([C:28]2[CH:33]=[CH:32][C:31]([CH3:34])=[CH:30][CH:29]=2)(=[O:27])=[O:26])[N:14]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 8058HexaneHCID 70297m-Chloroperbenzoic acidHCID 12857764Methyl 2-amino-6-[(p-tolylsulfonyl)oxy]-4-pyrimidinecarbamate

生成物 1

HCID 178502003HCID 178502003、化合物

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 6344Dichloromethane溶媒

実験手順

61.1 g (0.314 mol) of 88% m-chloroperbenzoic acid are added to a suspension of 50.7 g (0.15 mol) of methyl 2-amino-6-[(p-toluenesulfonyl)oxy]-4-pyrimidinecarbamate in 1800 ml of methylene chloride and 300 ml of methanol. The solution, which becomes clear after 2 hours, is stirred at room temperature overnight and thereafter warmed to 40° for 8 hours. 1800 ml of hexane are added to this solution and the mixture is cooled to 0° overnight, whereby there forms a crystalline precipitate which is filtered off under suction and dried. The mother liquor is concentrated to approximately 400 ml under reduced pressure, there being obtained a further crystalline precipitate of methyl 2-amino-6-[(p-toluenesulfonyl)oxy]-4-pyrimidinecarbamate-3-oxide of melting point 144°-145°.

後処理

  1. temperaturewarmed to 40° for 8 hours
  2. temperaturethe mixture is cooled to 0° overnight
  3. filtrationis filtered off under suction
  4. customdried
  5. concentrationThe mother liquor is concentrated to approximately 400 ml under reduced pressure, there

出典と根拠

ORDレコード
ord-dfca246f39804539b18f491087ed28e3
出典データセット
uspto-grants-1985_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04549019

反応ノート

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