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Potassium Carbonate → HCID 57971919、化合物

HRID 1921888
ノート
印刷プレビュー

反応式

HRID 1921888 の反応式
[F:1][C:2]1[CH:3]=[C:4]([CH:28]=[C:29]([F:42])[C:30]=1[O:31][Si:32]([CH:39]([CH3:41])[CH3:40])([CH:36]([CH3:38])[CH3:37])[CH:33]([CH3:35])[CH3:34])[CH2:5][CH:6](/[CH:19]=[CH:20]/[C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][C:22]=1[OH:27])[CH2:7][CH2:8][C:9]1[CH:18]=[CH:17][C:12]([C:13]([O:15][CH3:16])=[O:14])=[CH:11][CH:10]=1.[C:43]([C:47]1[CH:54]=[CH:53][C:50]([CH2:51]Br)=[CH:49][CH:48]=1)([CH3:46])([CH3:45])[CH3:44].C(=O)([O-])[O-].[K+].[K+]>C(#N)C>[C:43]([C:47]1[CH:48]=[CH:49][C:50]([CH2:51][O:27][C:22]2[CH:23]=[CH:24][CH:25]=[CH:26][C:21]=2/[CH:20]=[CH:19]/[CH:6]([CH2:5][C:4]2[CH:28]=[C:29]([F:42])[C:30]([O:31][Si:32]([CH:36]([CH3:38])[CH3:37])([CH:39]([CH3:41])[CH3:40])[CH:33]([CH3:34])[CH3:35])=[C:2]([F:1])[CH:3]=2)[CH2:7][CH2:8][C:9]2[CH:10]=[CH:11][C:12]([C:13]([O:15][CH3:16])=[O:14])=[CH:17][CH:18]=2)=[CH:53][CH:54]=1)([CH3:46])([CH3:44])[CH3:45]
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 3

HCID 11430Potassium CarbonateHCID 878361-(Bromomethyl)-4-(1,1-dimethylethyl)benzeneHCID 57971924Methyl E-4-[3-(3,5-difluoro-4-triisopropylsilanyloxybenzyl)-5-(2-hydroxyphenyl)pent-4-enyl]-benzoate

生成物 1

HCID 57971919HCID 57971919、化合物

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

A solution of 1.3 g (2.19 mmol) of methyl E4-[3-(3,5-difluoro-4-triisopropylsilanyloxybenzyl)-5-(2-hydroxyphenyl)pent-4-enyl]benzoate in 20 ml of dry acetonitrile is mixed with 600 mg (2.62 mmol) of 4-tert-butylbenzyl bromide and 450 mg (3.28 mmol) of anhydrous potassium carbonate and heated under reflux for 12 hours. The mixture is then concentrated to dryness. The residue is taken up in ethyl acetate, washed with water and saturated sodium chloride solution, dried over sodium sulfate and concentrated. The resulting crude product is purified by preparative HPLC. 780 mg (48% of theory) of a colorless oil are obtained.

後処理

  1. temperatureheated
  2. temperatureunder reflux for 12 hours
  3. concentrationThe mixture is then concentrated to dryness
  4. washwashed with water and saturated sodium chloride solution
  5. dry with materialdried over sodium sulfate
  6. concentrationconcentrated
  7. customThe resulting crude product is purified by preparative HPLC
  8. custom780 mg (48% of theory) of a colorless oil are obtained

出典と根拠

ORDレコード
ord-c49460fab9e647b9a5926ec9e26c0b0a
出典データセット
uspto-grants-2012_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08173704B2

反応ノート

読み込み中…

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