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

HRID 1034951

反応式

HRID 1034951 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

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)+.

後処理

  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

出典と根拠

ORDレコード
ord-9062883a5b4e4ff0b89f3a0092b22c31
出典データセット
uspto-grants-2013_10
特許番号
US08546368B2

関連ノート

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