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Tributylphenyltin → HCID 178472765、化合物

HRID 1746225
ノート
印刷プレビュー

反応式

HRID 1746225 の反応式
[CH2:1]([O:3][C:4](=[O:23])[CH2:5][NH:6][C:7]([C:9]1[C:10](=[O:22])[S:11][C:12]2[C:17]([C:18]=1[OH:19])=[CH:16][C:15]([Cl:20])=[CH:14][C:13]=2Br)=[O:8])[CH3:2].C([Sn](CCCC)(CCCC)[C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1)CCC>CN(C=O)C.C(OCC)(=O)C.O.C1(P([Pd-2](Cl)(Cl)P(C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>[CH2:1]([O:3][C:4](=[O:23])[CH2:5][NH:6][C:7]([C:9]1[C:10](=[O:22])[S:11][C:12]2[C:17]([C:18]=1[OH:19])=[CH:16][C:15]([Cl:20])=[CH:14][C:13]=2[C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1)=[O:8])[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 2

HCID 607632TributylphenyltinHCID 178472764HCID 178472764、化合物

生成物 1

HCID 178472765HCID 178472765、化合物収率 83.4%

試薬・触媒・溶媒 4

HCID 178418903HCID 178418903、化合物触媒HCID 962Water溶媒HCID 6228Dimethylformamide
溶媒
HCID 8857Ethyl Acetate溶媒

実験手順

[(8-Bromo-6-chloro-4-hydroxy-2-oxo-2H-thiochromene-3-carbonyl)-amino]-acetic acid ethyl ester (22(d)) (500 mg, 1.2 mmol) was dissolved in anhydrous DMF (5 mL). To the solution was added Tributyl-phenyl-stannane (467 uL, 1.43 mmol), bis(triphenylphosphino) palladium(II) dichloride (100 mg, 0.12 mmol) and 4A molecular sieves. The reaction was sealed and the solution was heated to 120 C for 45 minutes. The reaction was cooled, diluted with ethyl acetate (25 mL) and water (25 mL). The organic phase was separated, dried over magnesium sulfate and concentrated residue in vacuo. The residue was filtered through silica to provide the title compound (418 mg) which was used directly without further purification.

後処理

  1. customThe reaction was sealed
  2. temperaturethe solution was heated to 120 C for 45 minutes
  3. temperatureThe reaction was cooled
  4. customThe organic phase was separated
  5. dry with materialdried over magnesium sulfate and concentrated residue in vacuo
  6. filtrationThe residue was filtered through silica

出典と根拠

ORDレコード
ord-d6efe568be14485eb8002efd5dee1ae3
出典データセット
uspto-grants-2015_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09149476B2

反応ノート

読み込み中…

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