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Thionyl Chloride → HCID 86650204、化合物

HRID 1406420
ノート
印刷プレビュー

反応式

HRID 1406420 の反応式
[CH3:1][C:2]1[CH:16]=[CH:15][C:5]([CH2:6][N:7]2[CH:11]=[C:10]([C:12](O)=[O:13])[CH:9]=[N:8]2)=[CH:4][CH:3]=1.FC1C=CC(CN2C=C(C(O)=O)C=N2)=CC=1.S(Cl)([Cl:35])=O>C1(C)C=CC=CC=1>[CH3:1][C:2]1[CH:16]=[CH:15][C:5]([CH2:6][N:7]2[CH:11]=[C:10]([C:12]([Cl:35])=[O:13])[CH:9]=[N:8]2)=[CH:4][CH:3]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 24386Thionyl ChlorideHCID 196200321-((4-methylphenyl)methyl)-1H-pyrazole-4-carboxylic acidHCID 43565332HCID 43565332、化合物

生成物 1

HCID 86650204HCID 86650204、化合物

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

反応条件

温度
90 °C

実験手順

1-(4-Methyl-benzyl)-1H-pyrazole-4-carboxylic acid (0.618 g, 2.86 mmol), which had been prepared according to the protocol described for intermediate (6e), in Example 21, was stirred in toluene (20 mL) at RT and thionyl chloride (681 mg, 0.42 mL, 5.72 mmol) was added. The reaction mixture was slowly heated to 90° C. and heating continued for 3 hrs. After cooling the reaction was concentrated in vacuo. Toluene was added to the residue and concentrated in vacuo. This was repeated a further three times and the crude solid obtained was triturated using isohexane. The solids were separated by filtration washed with isohexane and dried in vacuo to afford 1-(4-methyl-benzyl)-1H-pyrazole-4-carbonyl chloride as a white solid, 0.67 g, quant.

後処理

  1. temperatureheating
  2. temperatureAfter cooling the reaction
  3. concentrationwas concentrated in vacuo
  4. additionToluene was added to the residue
  5. concentrationconcentrated in vacuo
  6. customthe crude solid obtained
  7. customwas triturated
  8. customThe solids were separated by filtration
  9. washwashed with isohexane
  10. customdried in vacuo

出典と根拠

ORDレコード
ord-87c384e2a8304abdab9dc93ef907696a
出典データセット
uspto-grants-2014_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08916591B2

反応ノート

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