Acetic Acid → HCID 86686093、化合物

HRID 1253448

反応式

HRID 1253448 の反応式
[CH3:1][O:2][C:3](=[O:18])[CH2:4][C:5]1[CH:9]=[C:8]([OH:10])[N:7]([C:11]2C=CC=CC=2Cl)[N:6]=1.C(O)(=O)C.[CH2:23]([C:27](OCC)(OCC)[O:28][CH2:29][CH3:30])[CH2:24][CH2:25][CH3:26]>C(#N)C>[CH3:1][O:2][C:3](=[O:18])[CH2:4][C:5]1=[N:6][N:7]([CH3:11])[C:8](=[O:10])/[C:9]/1=[C:27](\[O:28][CH2:29][CH3:30])/[CH2:23][CH2:24][CH2:25][CH3:26]

参加物

5

反応物 3

HCID 176Acetic AcidHCID 701951,1,1-TriethoxypentaneHCID 178499531HCID 178499531、化合物

生成物 1

HCID 86686093HCID 86686093、化合物

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

反応条件

温度
70 °C

実験手順

The mixture of the above obtained methyl (5-hydroxy-1-methyl-1H-pyrazol-3-yl)acetate (Compound of Formula (IV), 0.80 g) in acetonitrile (5 mL), glacial acetic acid (21 μl 0.1 equiv.) and BuC(OEt)3 (3 eq.) was heated at 70° C. for 1 h 15. The resulting red solution was concentrated in vacuo to afford a red syrup that was washed with cyclohexane and then dried in vacuo. Due to its relative instability, no further purification of methyl[(4Z)-4-(1-ethoxypentylidene)-1-methyl-5-oxo-4,5-dihydro-1H-pyrazol-3-yl]acetate was conducted (1.0 g, quantitative yield). MS (ESI+): 283.4; MS (ESI−): 281.3.

後処理

  1. additionThe mixture of the
  2. concentrationThe resulting red solution was concentrated in vacuo
  3. customto afford a red syrup that
  4. washwas washed with cyclohexane
  5. customdried in vacuo
  6. customDue to its relative instability, no further purification of methyl[(4Z)-4-(1-ethoxypentylidene)-1-methyl-5-oxo-4,5-dihydro-1H-pyrazol-3-yl]acetate

出典と根拠

ORDレコード
ord-8ddae73c475047ca9904455e40b28531
出典データセット
uspto-grants-2013_06
特許番号
US08455485B2

関連ノート

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