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Ethanol → HCID 67343100、化合物

HRID 1673474
ノート
印刷プレビュー

反応式

HRID 1673474 の反応式
Br[C:2]1[CH:7]=[CH:6][C:5]([OH:8])=[C:4]([Cl:9])[CH:3]=1.C(=O)([O-])O.[Na+].C(O)C.[C:18]([NH:26][C:27]1[CH:39]=[C:38](B2OC(C)(C)C(C)(C)O2)[CH:37]=[CH:36][C:28]=1[C:29]([O:31][C:32]([CH3:35])([CH3:34])[CH3:33])=[O:30])(=[O:25])[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1>[Pd].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(C)C=CC=CC=1.O>[C:18]([NH:26][C:27]1[CH:39]=[C:38]([C:2]2[CH:7]=[CH:6][C:5]([OH:8])=[C:4]([Cl:9])[CH:3]=2)[CH:37]=[CH:36][C:28]=1[C:29]([O:31][C:32]([CH3:34])([CH3:35])[CH3:33])=[O:30])(=[O:25])[C:19]1[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 702EthanolHCID 198594-Bromo-2-chlorophenolHCID 516892Sodium Bicarbonate2 回HCID 67342196HCID 67342196、化合物

生成物 1

HCID 67343100HCID 67343100、化合物

試薬・触媒・溶媒 3

HCID 11979704
Tetrakis(triphenylphosphine)palladium
触媒
HCID 962Water溶媒
HCID 1140Toluene溶媒2 回

実験手順

0.15 g of 4-bromo-2-chlorophenol, 0.18 g of sodium hydrogen carbonate, 0.6 mL of ethanol, 0.3 mL of water and 42 mg of tetrakis(triphenylphosphine) palladium(0) were added to 2.1 mL of toluene solution containing 0.37 g of tert-butyl 2-(benzamido)-4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)benzoate at room temperature, and the resulting mixture was heated to reflux for 4 hours. Toluene and a saturated sodium hydrogen carbonate aqueous solution were added after the reaction mixture was cooled to room temperature. The organic layer was separated and ethyl acetate was added after washed with a saturated sodium chloride aqueous solution and dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. Hexane was added to the obtained residue and a solid substance was separated by filtration to obtain tert-butyl 2-(benzamido)-4-(3-chloro-4-hydroxyphenyl)benzoate.

後処理

  1. temperaturethe resulting mixture was heated
  2. temperatureto reflux for 4 hours
  3. customThe organic layer was separated
  4. additionethyl acetate was added
  5. washafter washed with a saturated sodium chloride aqueous solution
  6. dry with materialdried over anhydrous magnesium sulfate
  7. customthe solvent was evaporated under reduced pressure
  8. additionHexane was added to the obtained residue
  9. customa solid substance was separated by filtration

出典と根拠

ORDレコード
ord-e4cc7abcc9354b6b867ad613b2a57ccb
出典データセット
uspto-grants-2011_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07999132B2

反応ノート

読み込み中…

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