Phloroglucinol → 3-Methyl-2-nitro-butyric acid ethyl ester

HRID 41065

反応式

HRID 41065 の反応式
[N:1]([O-:3])=[O:2].[Na+].C1(C=C(O)C=C(O)C=1)O.[CH2:14]([O:16][C:17](=[O:23])[CH:18](I)[CH:19]([CH3:21])[CH3:20])[CH3:15]>CN(C)C=O>[CH2:14]([O:16][C:17](=[O:23])[CH:18]([N+:1]([O-:3])=[O:2])[CH:19]([CH3:21])[CH3:20])[CH3:15]

参加物

5

反応物 3

HCID 359PhloroglucinolHCID 23668193Sodium NitriteHCID 57436974Ethyl 2-iodo-3-methylbutanoate

生成物 1

HCID 131404463-Methyl-2-nitro-butyric acid ethyl ester

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

実験手順

To an ice cooled solution of 5.31 g sodium nitrite and 8 g dried phloroglucinol in 70 ml dimethyl formamide is added a solution of 11.3 g 2-iodo-3-methyl-butyric acid ethyl ester in 30 ml dimethyl formamide. The solution is allowed to warm up to room temperature and is stirred over night. The solvent is removed at reduced pressure. The residue is dissolved in ethyl acetate and washed with water. The organic layer is dried and the solvent is removed. The title compound is obtained as an oil. MS: m/z (M+)=176.1

後処理

  1. customThe solvent is removed at reduced pressure
  2. dissolutionThe residue is dissolved in ethyl acetate
  3. washwashed with water
  4. customThe organic layer is dried
  5. customthe solvent is removed

出典と根拠

ORDレコード
ord-5d6e3ec387d34890bc6beb155f34c05e
出典データセット
uspto-grants-2013_09
特許番号
US08530493B2

関連ノート

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