Cyclohexanone → 4-cyclohex-1-enyl-5-methyl-2-phenyl-2H-pyrazol-3-ylamine

HRID 1034951

반응식

HRID 1034951 반응식
[NH2:1][C:2]1[N:6]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=2)[N:5]=[C:4]([CH3:13])[CH:3]=1.[C:14]1(=O)[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15]1>C(O)(=O)C>[C:14]1([C:3]2[C:4]([CH3:13])=[N:5][N:6]([C:7]3[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=3)[C:2]=2[NH2:1])[CH2:19][CH2:18][CH2:17][CH2:16][CH:15]=1

참가 물질

4

반응물 2

HCID 7967CyclohexanoneHCID 708015-Amino-3-methyl-1-phenylpyrazole

생성물 1

HCID 694762524-cyclohex-1-enyl-5-methyl-2-phenyl-2H-pyrazol-3-ylamine수율 74.4%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

A solution of 5-amino-3-methyl-1-phenylpyrazole (8.66 g, 50 mmol) in acetic acid (70 mL) was treated with cyclohexanone (10.6 mL, 100 mmol) at ambient temperature for 40 hours. The volatiles were removed and the residue diluted with water and 10% sodium hydroxide added until the pH=12. The mixture was stirred with 10 mL of hexane for 30 minutes and the solid collected by filtration, washed with water and hexane and dried to give 9.43 g (74%) of the title compound. MS (DCI): m/z 254 (M+H)+.

후처리

  1. customThe volatiles were removed
  2. additionthe residue diluted with water and 10% sodium hydroxide
  3. additionadded until the pH=12
  4. filtrationthe solid collected by filtration
  5. washwashed with water and hexane
  6. customdried

출처 및 근거

ORD 기록
ord-9062883a5b4e4ff0b89f3a0092b22c31
출처 데이터셋
uspto-grants-2013_10
특허 번호
US08546368B2

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