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3-Nitrophenylboronic Acid → 2-Ethyl-7-(3-nitro-phenyl)-4H-benzo[1,4]thiazin-3-one

HRID 1007100
ノート
印刷プレビュー

反応式

HRID 1007100 の反応式
Br[C:2]1[CH:14]=[CH:13][C:5]2[NH:6][C:7](=[O:12])[CH:8]([CH2:10][CH3:11])[S:9][C:4]=2[CH:3]=1.[N+:15]([C:18]1[CH:19]=[C:20](B(O)O)[CH:21]=[CH:22][CH:23]=1)([O-:17])=[O:16].C(=O)([O-])[O-].[K+].[K+]>C(COC)OC.C(O)C.O.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[CH2:10]([CH:8]1[C:7](=[O:12])[NH:6][C:5]2[CH:13]=[CH:14][C:2]([C:22]3[CH:21]=[CH:20][CH:19]=[C:18]([N+:15]([O-:17])=[O:16])[CH:23]=3)=[CH:3][C:4]=2[S:9]1)[CH3:11]
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 3

HCID 16773-Nitrophenylboronic AcidHCID 11430Potassium CarbonateHCID 226677487-bromo-2-ethyl-4H-benzo[1,4]thiazin-3-one

生成物 1

HCID 98833222-Ethyl-7-(3-nitro-phenyl)-4H-benzo[1,4]thiazin-3-one収率 7.4%

試薬・触媒・溶媒 4

HCID 178418397HCID 178418397、化合物触媒
HCID 702
Ethanol
溶媒
HCID 962Water溶媒2 回
HCID 80711,2-Dimethoxyethane溶媒

実験手順

A solution of 7-bromo-2-ethyl-4H-benzo[1,4]thiazin-3-one (2 g, 7.3 mmol), 3-nitrophenyl boronic acid (1.22 g, 7.3 mmol), potassium carbonate (3 g, 22 mmol), and tetrakis(triphenylphosphine)palladium(0) (0.84 g, 0.72 mmol) in dimethoxyethane (100 ml), ethanol (25 ml), and water (25 ml) was heated to reflux for 6 hours. After cooling to room temperature, the mixture was diluted with water and extracted with EtOAc (3×40 mL). The combined organic extracts were washed with water, then brine, dried (MgSO4) and evaporated. The residue was recrystallized from ethanol to afford the title compound as tan crystals (0.17 g, 7.3%): mp 180° C.; MS (EI) m/z 314 (M+).

後処理

  1. temperatureto reflux for 6 hours
  2. extractionextracted with EtOAc (3×40 mL)
  3. washThe combined organic extracts were washed with water
  4. dry with materialbrine, dried (MgSO4)
  5. customevaporated
  6. customThe residue was recrystallized from ethanol

出典と根拠

ORDレコード
ord-35771439dda347bd803c68a50697ec29
出典データセット
uspto-grants-2004_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06794373B2

反応ノート

読み込み中…

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