Triethylamine → HCID 68537700、化合物

HRID 1931407ノート

反応式

HRID 1931407 の反応式
[CH2:1]([O:3][C:4](=[O:13])[CH2:5][C:6]([CH3:12])([CH3:11])[C:7](=O)[CH2:8]Br)[CH3:2].[F:14][C:15]([F:26])([F:25])[C:16]1[CH:24]=[CH:23][C:19]([C:20]([NH2:22])=[S:21])=[CH:18][CH:17]=1.C(N(CC)CC)C>C1(C)C=CC=CC=1>[CH2:1]([O:3][C:4](=[O:13])[CH2:5][C:6]([CH3:12])([C:7]1[N:22]=[C:20]([C:19]2[CH:18]=[CH:17][C:16]([C:15]([F:25])([F:14])[F:26])=[CH:24][CH:23]=2)[S:21][CH:8]=1)[CH3:11])[CH3:2]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 2724583Ethyl 5-bromo-3,3-dimethyl-4-oxopentanoateHCID 27348234-(Trifluoromethyl)thiobenzamide

生成物 1

HCID 68537700HCID 68537700、化合物

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

500 mg (1.99 mmol) of 5-bromo-3,3-dimethyl-4-oxo-pentanoic acid ethyl ester, 408.6 mg (1.99 mmol) of 4-trifluoromethyl-thiobenzamide and 403 mg (3.98 mmol) of triethylamine in 10 ml of toluene were stirred at 80° C. for 2 h. After evaporation, water and dichloromethane were added, the organic phase was separated, washed with water, dried, and evaporated. The product was purified by chromatography (silica gel, n-heptane/ethyl acetate 8:1). Yield: 498.5 mg.

後処理

  1. customAfter evaporation, water and dichloromethane
  2. additionwere added
  3. customthe organic phase was separated
  4. washwashed with water
  5. customdried
  6. customevaporated
  7. customThe product was purified by chromatography (silica gel, n-heptane/ethyl acetate 8:1)

出典と根拠

ORDレコード
ord-9c784b38cb46447dbea445840834b450
出典データセット
uspto-grants-2012_05
特許番号
US08188291B2

反応ノート

読み込み中…