Acrylic Acid → N-[3-(Dimethylamino)propyl]-N-[(nonafluorobutyl)sulfonyl]-beta-alanine

HRID 129354

反応式

HRID 129354 の反応式
[C:1]([OH:5])(=[O:4])[CH:2]=[CH2:3].[C:6]([S:19]([NH:22][CH2:23][CH2:24][CH2:25][N:26]([CH3:28])[CH3:27])(=[O:21])=[O:20])([C:9]([C:12]([C:15]([F:18])([F:17])[F:16])([F:14])[F:13])([F:11])[F:10])([F:8])[F:7].C1C2NC3C(=CC=CC=3)SC=2C=CC=1.C(OCCOCCO)CCC>O>[C:6]([S:19]([N:22]([CH2:23][CH2:24][CH2:25][N:26]([CH3:27])[CH3:28])[CH2:3][CH2:2][C:1]([OH:5])=[O:4])(=[O:20])=[O:21])([C:9]([C:12]([C:15]([F:16])([F:17])[F:18])([F:14])[F:13])([F:11])[F:10])([F:8])[F:7]

参加物

6

反応条件

温度
125 °C

実験手順

An acrylic acid Michael addition reaction was then run according to the general procedure given in U.S. Pat. No. 5,144,069 (Stern et al.). 50 g (0.12 mole) of the purified C4F9SO2N(H)C3H6N(CH3)2, 16.4 g (0.23 mole) of acrylic acid and 0.2 g of phenothiazine (free radical polymerization inhibitor) were added to a 250-mL three-neck flask equipped with an air stirrer and thermometer. The resulting mixture was heated to 125° C. and was allowed to react for 6 hours. After this reaction period, a positive solubility check of the product in water of pH 7 indicated that the Michael addition reaction was essentially complete. While still mixing, a solvent blend of 18 g of diethylene glycol monobutyl ether and 42 g of deionized water was added and the mixture was allowed to cool to room temperature. The water solubility test was run again with the same positive result, showing good conversion to the desired Michael addition product, C4F9SO2N(C2H4COOH)C3H6 (CH3)2.

後処理

  1. customequipped with an air stirrer
  2. customto react for 6 hours
  3. customAfter this reaction period
  4. additionWhile still mixing
  5. temperatureto cool to room temperature

出典と根拠

ORDレコード
ord-6db07f2762984316b90d6f5c14a17a70
出典データセット
uspto-grants-1995_11
特許番号
US05468353

関連ノート

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