Butylamine → HCID 21091498、化合物

HRID 1348598ノート

反応式

HRID 1348598 の反応式
CC1(C)[O:7][C:6](=[O:8])[C:5]([CH3:10])([CH3:9])[C:4](=[O:11])O1.[CH2:13]([NH2:17])[CH2:14][CH2:15][CH3:16]>C(N(CC)C(C)C)(C)C>[CH2:13]([NH:17][C:4](=[O:11])[C:5]([CH3:9])([CH3:10])[C:6]([OH:7])=[O:8])[CH2:14][CH2:15][CH3:16]

参加物

4

反応物 2

HCID 8007ButylamineHCID 3808172,2,5,5-Tetramethyl-1,3-dioxane-4,6-dione

生成物 1

HCID 21091498HCID 21091498、化合物収率 60%

試薬・触媒・溶媒 1

HCID 81531Diisopropylethylamine溶媒

実験手順

1.72 g (10 mmol) —2,2,5,5-Tetramethyl-[1,3]dioxane-4,6-dione and 1.02 ml butylamine were stirred in 7 ml N,N-diisopropyl-ethylamine for 18 hours at room temperature. The excess N,N-diisopropyl-ethylamine was decanted and the residue was extracted with 1N aqueous hydrochloric acid/ethylacetate. The ethylacetate phase was washed with 1N aqueous hydrochloric acid, brine and was dried over sodiumsulfate. Evaporation of the solvent and recrystallisation from dichloromethane/heptane yielded 60% N-butyl-2,2-dimethyl-malonamic acid as white solid, MS m/e (%): 188.4 (M+H+, 100).

後処理

  1. customThe excess N,N-diisopropyl-ethylamine was decanted
  2. extractionthe residue was extracted with 1N aqueous hydrochloric acid/ethylacetate
  3. washThe ethylacetate phase was washed with 1N aqueous hydrochloric acid, brine
  4. dry with materialwas dried over sodiumsulfate
  5. customEvaporation of the solvent and recrystallisation from dichloromethane/heptane

出典と根拠

ORDレコード
ord-ee1e9fabe45c43d4a30c1f566073633e
出典データセット
uspto-grants-2007_05
特許番号
US07211573B2

反応ノート

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