Diethylenetriamine → 2,2,2-trifluoro-N-[2-[2-[(2,2,2-trifluoroacetyl)amino]ethylamino]ethyl]acetamide

HRID 439639

反応式

HRID 439639 の反応式
C(O[C:4](=[O:9])[C:5]([F:8])([F:7])[F:6])C.[NH2:10][CH2:11][CH2:12][NH:13][CH2:14][CH2:15][NH2:16]>O1CCCC1>[F:6][C:5]([F:8])([F:7])[C:4]([NH:10][CH2:11][CH2:12][NH:13][CH2:14][CH2:15][NH:16][C:4](=[O:9])[C:5]([F:6])([F:7])[F:8])=[O:9]

参加物

4

反応物 2

HCID 8111DiethylenetriamineHCID 9794Ethyl trifluoroacetate

生成物 1

HCID 3887782,2,2-trifluoro-N-[2-[2-[(2,2,2-trifluoroacetyl)amino]ethylamino]ethyl]acetamide

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

113.3 g (790 mmol) of trifluoroacetic acid ethyl ester is instilled in a solution of 41.14 g (390 mmol) of 1,4,7-triazaheptane in 350 ml of tetrahydrofuran at 0° C. and under nitrogen. It is allowed to stir overnight at room temperature, concentrated by evaporation in a vacuum. The remaining oil is crystallized from hexane. Yield: 115 g (99.9% of theory) Melting point: 68°-70° C. Elementary analysis: Cld: C 32.55 H 3.76 F 38.62 N 14.24 Fnd: C 32.63 H 3.75 F 38.38 N 14.19

後処理

  1. concentrationconcentrated by evaporation in a vacuum
  2. customThe remaining oil is crystallized from hexane

出典と根拠

ORDレコード
ord-d92f6b3a84314d6c9a8d07e55ec5c76e
出典データセット
uspto-grants-1996_05
特許番号
US05514810

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