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Hydrochloric Acid → HCID 178498937、化合物

HRID 1746201
ノート
印刷プレビュー

反応式

HRID 1746201 の反応式
[CH3:1][O:2][C:3]([C:5]1[C:6](=[O:17])[S:7][C:8]2[C:13]([C:14]=1[OH:15])=[CH:12][CH:11]=[C:10](Br)[CH:9]=2)=[O:4].[CH2:18]([B-](F)(F)F)[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1.[K+].C([O-])([O-])=O.[Cs+].[Cs+].Cl>C1COCC1.O.Cl[Pd](Cl)([P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)[P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1>[CH3:1][O:2][C:3]([C:5]1[C:6](=[O:17])[S:7][C:8]2[C:13]([C:14]=1[OH:15])=[CH:12][CH:11]=[C:10]([CH2:18][C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)[CH:9]=2)=[O:4]
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 313Hydrochloric AcidHCID 10796Cesium carbonateHCID 23692459Potassium benzyltrifluoroboranuideHCID 178498916HCID 178498916、化合物

生成物 1

HCID 178498937HCID 178498937、化合物収率 43.3%

試薬・触媒・溶媒 3

HCID 178418476
HCID 178418476、化合物
触媒
HCID 962Water溶媒2 回
HCID 8028Tetrahydrofuran溶媒

実験手順

To a mixture of 7-bromo-4-hydroxy-2-oxo-2H-thiochromene-3-carboxylic acid methyl ester (Example 5 e) (220 mg, 0.70 mmol) in THF (8 mL) was added potassium benzyltrifluoroborate (138 mg, 0.70 mmol), Cs2CO3 (682 mg, 2.09 mmol), PdCl2(PPh3)2 (49 mg, 0.07 mmol) and then water (2 mL). The resulting mixture was refluxed overnight (18 h). After cooling, the reaction mixture was diluted with water (75 mL) and acidified using 1 N HCl to pH 4. The precipitate was collected, rinsed with water and the solid dissolved in CH2Cl2. The CH2Cl2 solution was dried over MgSO4, filtered, concentrated and the crude product purified by silica gel chromatography (5%-100% EtOAc/CH2Cl2) to provide 7-benzyl-4-hydroxy-2-oxo-2H-thiochromene-3-carboxylic acid methyl ester (99 mg). 1H NMR (200 MHz, CDCl3): δ (ppm)=15.2 (s, 1H), 8.25 (d, J=8.2 Hz, 1H), 7.36-7.16 (m, 7H), 4.04 (s, 2H), 4.00 (s, 3H).

後処理

  1. temperatureThe resulting mixture was refluxed overnight (18 h)
  2. temperatureAfter cooling
  3. customThe precipitate was collected
  4. washrinsed with water
  5. dissolutionthe solid dissolved in CH2Cl2
  6. dry with materialThe CH2Cl2 solution was dried over MgSO4
  7. filtrationfiltered
  8. concentrationconcentrated
  9. customthe crude product purified by silica gel chromatography (5%-100% EtOAc/CH2Cl2)

出典と根拠

ORDレコード
ord-42bccdc23f0845308258874d7ca93711
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

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