Ammonium trifluoroacetate → HCID 178432621、化合物

HRID 2367399ノート

反応式

HRID 2367399 の反応式
[CH3:1][CH:2]([NH:11][C:12]([CH:14]1[O:19][CH2:18][CH2:17][N:16]([CH2:20][C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)[CH2:15]1)=O)[C:3](=O)[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1.FC(F)(F)C([O-])=O.[NH4+:34]>>[CH3:1][C:2]1[N:11]=[C:12]([CH:14]2[O:19][CH2:18][CH2:17][N:16]([CH2:20][C:21]3[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=3)[CH2:15]2)[NH:34][C:3]=1[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1

参加物

3

反応物 2

HCID 2724268Ammonium trifluoroacetateHCID 58504388N-(1-Methyl-2-oxo-2-phenylethyl)-4-(phenylmethyl)-2-morpholinecarboxamide

生成物 1

HCID 178432621HCID 178432621、化合物収率 97.5%

反応条件

温度
150 °C

実験手順

A mixture of N-(1-methyl-2-oxo-2-phenylethyl)-4-(phenylmethyl)-2-morpholinecarboxamide (1.3 g, 3.69 mmol) and ammonium trifluoroacetate (2.417 g, 18.44 mmol) was stirred for 0.75 hours at 150° C. The LCMS indicated that the starting material was consumed. The desired product was contained in the residue. Water (150 mL) was added to the residue, and the resulting mixture was extracted with EtOAc (3×100 mL). The organics were dried (Na2SO4), filtered, and evaporated to afford the title compound (1.2 g) as a brown oil. LC-MS (ES) m/z=334 [M+H]+.

後処理

  1. customwas consumed
  2. additionWater (150 mL) was added to the residue
  3. extractionthe resulting mixture was extracted with EtOAc (3×100 mL)
  4. dry with materialThe organics were dried (Na2SO4)
  5. filtrationfiltered
  6. customevaporated

出典と根拠

ORDレコード
ord-6b4055e68b5042bcbca5314743d8fc31
出典データセット
uspto-grants-2014_04
特許番号
US08697685B2

反応ノート

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