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Diethylamine → 2,2,2-TRIFLUOROET AMINE,N,N-DIET

HRID 2119264
ノート
印刷プレビュー

反応式

HRID 2119264 の反応式
[CH2:1]([NH:3][CH2:4][CH3:5])[CH3:2].C(=O)([O-])[O-].[K+].[K+].[F:12][C:13]([F:24])([F:23])[CH2:14]OS(C(F)(F)F)(=O)=O>O>[CH2:1]([N:3]([CH2:4][CH3:5])[CH2:14][C:13]([F:24])([F:23])[F:12])[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 8021DiethylamineHCID 11430Potassium CarbonateHCID 803662,2,2-Trifluoroethyl trifluoromethanesulfonate

生成物 1

HCID 135100982,2,2-TRIFLUOROET AMINE,N,N-DIET

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Diethyl 2,2,2-trifluoroethylamine was prepared as follows. Into a flask were placed diethylamine (5.5 g) and potassium carbonate (10.0 g). 2,2,2-Trifluoroethyl-trifluoromethanesulfonate (12 g) was slowly added to the flask. Heat was evolved. After addition, the reaction mixture was stirred at room temperature overnight. Approximately 100 mL of water was added and the organic layer was separated and dried over MgSO4. The organic liquid was distilled to receive a fraction (a clear liquid 7.25 g) at 88-89° C. under normal pressure. The clear liquid was sampled and analyzed by 1H and 19F NMR. 1H NMR: δ3.56 (q, 2H, J=9 Hz), 2.65 (q, 2H, J=7 Hz), 1.10 (t, 3H, J=7H); ·F NMR: δ−68.13 (t, 3F, J=9 Hz).

後処理

  1. customInto a flask were placed
  2. temperatureHeat
  3. additionAfter addition
  4. customthe organic layer was separated
  5. dry with materialdried over MgSO4
  6. distillationThe organic liquid was distilled
  7. customat 88-89° C.
  8. aliquotThe clear liquid was sampled

出典と根拠

ORDレコード
ord-efff28170c394105a79719e9fb428be0
出典データセット
uspto-grants-2004_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06685793B2

反応ノート

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