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

HRID 41065

반응식

HRID 41065 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

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

후처리

  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

출처 및 근거

ORD 기록
ord-5d6e3ec387d34890bc6beb155f34c05e
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08530493B2

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