Water → 1-benzylazetidine-3,3-dicarboxylic Acid

HRID 868183

反応式

HRID 868183 の反応式
BrBr.[CH2:3]([N:10]1[CH2:13][C:12]([CH2:16][OH:17])([CH2:14][OH:15])[CH2:11]1)[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1.[OH-:18].[Na+].[OH2:20]>S([O-])([O-])(=O)=O.[Ni+2]>[CH2:3]([N:10]1[CH2:13][C:12]([C:14]([OH:20])=[O:15])([C:16]([OH:18])=[O:17])[CH2:11]1)[C:4]1[CH:5]=[CH:6][CH:7]=[CH:8][CH:9]=1

参加物

6

反応物 4

HCID 962WaterHCID 14798Sodium HydroxideHCID 24408BromineHCID 20164320[1-Benzyl-3-(hydroxymethyl)azetidin-3-YL]methanol

生成物 1

HCID 113108851-benzylazetidine-3,3-dicarboxylic Acid

試薬・触媒・溶媒 1

HCID 24586Nickel Sulfate触媒

実験手順

Bromine (10.6 g) was slowly added at 20° C. over 8 hours to a mixture of N-benzyl-3,3-bis(hydroxymethyl)azetidine (2.1 g) in water (50 ml) containing sodium hydroxide (9.3 g) and nickel chloride 6.0 aq. (1.5 g). After stirring overnight, the green precipitate of nickel hydroxide was filtered off, and the filtrate evaporated to dryness. The residue was boiled in ethanol, and the insoluble material (desired product as sodium salt and sodium bromide) separated and worked up to yield the N-benzyl-azetidine-3,3-dicarboxylic acid.

後処理

  1. filtrationthe green precipitate of nickel hydroxide was filtered off
  2. customthe filtrate evaporated to dryness
  3. customthe insoluble material (desired product as sodium salt and sodium bromide) separated

出典と根拠

ORDレコード
ord-838be3ff0e684522a9c780bbcef962f4
出典データセット
uspto-grants-1988_10
特許番号
US04778577

関連ノート

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