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Pyrazole → HCID 69136279、化合物

HRID 1836864
ノート
印刷プレビュー

反応式

HRID 1836864 の反応式
[CH3:1][O:2][C:3](=[O:28])[C:4]1[CH:9]=[CH:8][C:7](/[CH:10]=[CH:11]/[C:12]2[C:21]([CH2:22]Br)=[CH:20][C:19]3[C:18]([CH3:25])([CH3:24])[CH2:17][CH2:16][C:15]([CH3:27])([CH3:26])[C:14]=3[CH:13]=2)=[CH:6][CH:5]=1.[NH:29]1[CH:33]=[CH:32][CH:31]=[N:30]1>CN1CCCC1.[Cl-].[Na+].O>[CH3:1][O:2][C:3](=[O:28])[C:4]1[CH:9]=[CH:8][C:7]([CH:10]=[CH:11][C:12]2[C:21]([CH2:22][N:29]3[CH:33]=[CH:32][CH:31]=[N:30]3)=[CH:20][C:19]3[C:18]([CH3:25])([CH3:24])[CH2:17][CH2:16][C:15]([CH3:27])([CH3:26])[C:14]=3[CH:13]=2)=[CH:6][CH:5]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 1048PyrazoleHCID 23498883(E)-methyl-4-[2-(3-bromomethyl-5,5,8,8-tetramethyl-5,6,7,8-tetrahydro-naphthalen-2-yl)vinyl]benzoate

生成物 1

HCID 69136279HCID 69136279、化合物収率 83%

試薬・触媒・溶媒 2

HCID 84541-Methylpyrrolidine溶媒HCID 57417360Sodium chloride; water溶媒

実験手順

A mixture of 2.0 g (4.5 mmol) of (E)-methyl-4-[2-(3-bromomethyl-5,5,8,8-tetramethyl-5,6,7,8-tetrahydro-naphthalen-2-yl)vinyl]benzoate and 0.65 g (9.5 mmol) of pyrazole in 15 mL of N-methyl pyrrolidine was heated at 100°. After 2 hours, the reaction mixture was cooled to room temperature, poured into brine and extracted with ethyl acetate. The organic extracts were washed with brine, dried over sodium sulfate and concentrated under reduced pressure. The residue was stirred with hexane and the product was filtered off, washed with hexane and dried to give 1.6 g (83%) of methyl-4-[2-(5,5,8,8-Tetramethyl-3-pyrazol-1-ylmethyl-5,6,7,8-tetrahydro-naphthalen-2-yl)vinyl]benzoate (M+=429).

後処理

  1. temperaturewas heated at 100°
  2. extractionextracted with ethyl acetate
  3. washThe organic extracts were washed with brine
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated under reduced pressure
  6. filtrationthe product was filtered off
  7. washwashed with hexane
  8. customdried

出典と根拠

ORDレコード
ord-1e5aab86749748afab1ca9e33bbb9781
出典データセット
uspto-grants-2004_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06777418B2

反応ノート

読み込み中…

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