Potassium Iodide → 1040718-40-8

HRID 1695209노트

반응식

HRID 1695209 반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[NH:13][N:12]=[C:11]([NH:14][C:15](=[O:21])[CH2:16][CH2:17][CH2:18][CH2:19]Br)[CH:10]=2)=[CH:5][CH:4]=1.C(=O)([O-])[O-].[K+].[K+].[I-].[K+].[C:30]([N:33]1[CH2:39][CH2:38][CH2:37][NH:36][CH2:35][CH2:34]1)(=[O:32])[CH3:31].IC1C=CNN=1>CC(C)=O>[C:30]([N:33]1[CH2:39][CH2:38][CH2:37][N:36]([CH2:19][CH2:18][CH2:17][CH2:16][C:15]([NH:14][C:11]2[CH:10]=[C:9]([C:6]3[CH:7]=[CH:8][C:3]([O:2][CH3:1])=[CH:4][CH:5]=3)[NH:13][N:12]=2)=[O:21])[CH2:35][CH2:34]1)(=[O:32])[CH3:31]

참가 물질

7

반응물 5

HCID 4875Potassium IodideHCID 11430Potassium CarbonateHCID 4186202N-AcetylhomopiperazineHCID 577800445-bromo-N-(5-(4-methoxyphenyl)-1H-pyrazol-3-yl)pentanamideHCID 178506555HCID 178506555, 화합물

생성물 1

HCID 248605821040718-40-8

시약·촉매·용매 1

HCID 180Acetone용매

반응 조건

온도
27.5 °C

실험 절차

To a cylindrical, jacketed 3 L reactor equipped with nitrogen inerting, agitator, condenser/distillation head, and temperature control, 5-bromo-pentanoic acid [5-(4-methoxy-phenyl)-1H-pyrazol-3-yl]amide (0.15 kg, 0.426 mol), potassium carbonate (0.059 kg, 0.426 mol), potassium iodide (0.071 kg, 0.426 mol), and acetone (1.18 kg, 1.5 L) were added (at 20° C.) to form a white mixture. The mixture was stirred (235 rpm) at 25-30° C. for a minimum of 15 min. N-acetylhomopiperazine (0.062 kg, 0.057 L, 0.434 mol) was added via addition funnel to the reactor over a minimum of 45 min., maintaining the temperature in the range of 25-30° C. The addition funnel was rinsed with 0.05 L acetone. A white mixture persisted. The mixture was stirred (235 rpm) in the range of 25-30° C. for a minimum of 16 h, forming a white/yellow mixture. The reaction progress was monitored by HPLC and was considered complete when there was ≦2% of the starting material (bromopyrazole) and ≦2% of the iodopyrazole present.

후처리

  1. additionwere added (at 20° C.)
  2. customto form a white mixture
  3. temperaturemaintaining the temperature in the range of 25-30° C
  4. washThe addition funnel was rinsed with 0.05 L acetone
  5. stirringThe mixture was stirred (235 rpm) in the range of 25-30° C. for a minimum of 16 h
  6. customforming a white/yellow mixture

출처 및 근거

ORD 기록
ord-00121884c5954f27a6912dcc169de615
출처 데이터셋
uspto-grants-2012_04
특허 번호
US08163729B2

반응 노트

불러오는 중…