Water → 5-[2-(4-Chlorophenyl)-1,3-dioxolan-2-yl]-3-(3-methoxyphenyl)-2,1-benzisoxazole

HRID 564828ノート

反応式

HRID 564828 の反応式
[OH-].[Na+].[CH3:3][O:4][C:5]1[CH:6]=[C:7]([CH2:11][C:12]#N)[CH:8]=[CH:9][CH:10]=1.[Cl:14][C:15]1[CH:20]=[CH:19][C:18]([C:21]2([C:26]3[CH:31]=C[C:29]([N+:32]([O-])=[O:33])=[CH:28][CH:27]=3)[O:25][CH2:24][CH2:23][O:22]2)=[CH:17][CH:16]=1.O>CO>[Cl:14][C:15]1[CH:16]=[CH:17][C:18]([C:21]2([C:26]3[CH:27]=[CH:28][C:29]4[C:12]([CH:31]=3)=[C:11]([C:7]3[CH:8]=[CH:9][CH:10]=[C:5]([O:4][CH3:3])[CH:6]=3)[O:33][N:32]=4)[O:22][CH2:23][CH2:24][O:25]2)=[CH:19][CH:20]=1

参加物

6

反応物 4

HCID 962WaterHCID 14798Sodium HydroxideHCID 88310(3-Methoxyphenyl)acetonitrileHCID 154896262-(4-Chlorophenyl)-2-(4-nitrophenyl)-1,3-dioxolane

生成物 1

HCID 227143745-[2-(4-Chlorophenyl)-1,3-dioxolan-2-yl]-3-(3-methoxyphenyl)-2,1-benzisoxazole収率 90%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Sodium hydroxide (16.4 g) and (3-methoxyphenyl)acetonitrile (20.6 ml) were added at room temperature to a solution of interm. (5-a) (25 g) in methanol (100 ml) and the mixture was stirred at room temperature overnight. Water was added, the precipitate was filtered off, washed with cold methanol and dried. The product was used without further purification, yielding 30 g (90%) of 5-[2-(4-chlorophenyl)-1,3-dioxolan-2-yl]-3-(3-methoxyphenyl)-2,1-benzisoxazole (interm. 5-b).

後処理

  1. filtrationthe precipitate was filtered off
  2. washwashed with cold methanol
  3. customdried
  4. customThe product was used without further purification

出典と根拠

ORDレコード
ord-5639f7ad85ba4f1896e42f1820058417
出典データセット
uspto-grants-2001_01
特許番号
US06169096A

反応ノート

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