Acetic Acid → HCID 86686093, 화합물

HRID 1253448

반응식

HRID 1253448 반응식
[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]

참가 물질

5

반응물 3

HCID 176Acetic AcidHCID 701951,1,1-TriethoxypentaneHCID 178499531HCID 178499531, 화합물

생성물 1

HCID 86686093HCID 86686093, 화합물

시약·촉매·용매 1

HCID 6342Acetonitrile용매

반응 조건

온도
70 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-8ddae73c475047ca9904455e40b28531
출처 데이터셋
uspto-grants-2013_06
특허 번호
US08455485B2

연결된 노트

불러오는 중…