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Tri-o-tolylphosphine → tert-butyl (3E)-4-(3-amino-4-phenylphenyl)-3-butenoate

HRID 1518632
ノート
印刷プレビュー

反応式

HRID 1518632 の反応式
[C:1]1([C:7]2[CH:13]=[C:12](Br)[CH:11]=[CH:10][C:8]=2[NH2:9])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[C:15]([O:19][C:20](=[O:24])[CH2:21][CH:22]=[CH2:23])([CH3:18])([CH3:17])[CH3:16].C1(C)C=CC=CC=1P(C1C=CC=CC=1C)C1C=CC=CC=1C.C(N(C(C)C)CC)(C)C>CN(C)C=O.C([O-])(=O)C.[Pd+2].C([O-])(=O)C>[NH2:9][C:8]1[CH:10]=[C:11](/[CH:23]=[CH:22]/[CH2:21][C:20]([O:19][C:15]([CH3:18])([CH3:17])[CH3:16])=[O:24])[CH:12]=[CH:13][C:7]=1[C:1]1[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=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

7

反応物 4

HCID 80271Tri-o-tolylphosphineHCID 81531DiisopropylethylamineHCID 2295504-Bromo-2-phenylanilineHCID 639778tert-Butyl 3-Butenoate

生成物 1

HCID 66597453tert-butyl (3E)-4-(3-amino-4-phenylphenyl)-3-butenoate収率 78.8%

試薬・触媒・溶媒 2

HCID 167845
palladium(II) acetate
触媒
HCID 6228Dimethylformamide溶媒

反応条件

温度
90 °C

実験手順

2-Phenyl-4-bromoaniline (564.7 mg, 2.28 mmol) was dissolved in N,N-dimethylformamide (25 mL) and, at room temperature, thereto were added tert-butyl-3-butenoate (582.5 mg, 4.10 mmol), tri-(o-tolyl)phosphine (1.87 g, 6.16 mmol), and diisopropylethylamine (0.78 mL, 4.56 mmol). The reaction mixture was deaerated, palladium acetate (67.4 mg, 0.30 mmol) was added, and the mixture was deaerated again. After stirring at 90° C. overnight, the reaction mixture was filtered through celite and washed with ethyl acetate (120 mL). The organic layer was washed with a saturated aqueous solution of sodium chloride (50 mL), thereafter dried over sodium sulfate, filtered, and concentrated under reduced pressure. The residue was purified by a silica gel column to obtain tert-butyl (3E)-4-(3-amino-4-phenylphenyl)-3-butenoate (555.8 mg).

後処理

  1. filtrationthe reaction mixture was filtered through celite
  2. washwashed with ethyl acetate (120 mL)
  3. washThe organic layer was washed with a saturated aqueous solution of sodium chloride (50 mL)
  4. dry with materialdried over sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure
  7. customThe residue was purified by a silica gel column

出典と根拠

ORDレコード
ord-cb84ccb8ef9742119fd83111ef388a03
出典データセット
uspto-grants-2015_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09072734B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート