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Tricyclohexylphosphine → 3-benzenesulfonyl-3H-indene-1-carboxylic acid ethyl ester

HRID 10081
ノート
印刷プレビュー

反応式

HRID 10081 の反応式
C1(P(C2CCCCC2)C2CCCCC2)CCCCC1.CC(C)([O-])C.[Na+].[CH2:26]([O:28][C:29](=[O:35])[CH:30]=[CH:31]OCC)[CH3:27].[C:36]1([S:42]([CH2:45][C:46]2[CH:51]=[CH:50][CH:49]=[CH:48][C:47]=2Br)(=[O:44])=[O:43])[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=1.P([O-])(O)(O)=O.[K+]>O1CCCC1.C(OC)(C)(C)C.C([O-])(=O)C.[Pd+2].C([O-])(=O)C>[CH2:26]([O:28][C:29]([C:30]1[C:47]2[C:46](=[CH:51][CH:50]=[CH:49][CH:48]=2)[CH:45]([S:42]([C:36]2[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=2)(=[O:44])=[O:43])[CH:31]=1)=[O:35])[CH3:27]
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

9

反応物 5

HCID 75806TricyclohexylphosphineHCID 221780Ethyl 3-ethoxy-2-propenoateHCID 516951Monobasic potassium phosphateHCID 113359052-Bromobenzyl Phenyl SulfoneHCID 23676156Sodium t-butoxide

生成物 1

HCID 99234833-benzenesulfonyl-3H-indene-1-carboxylic acid ethyl ester収率 85%

試薬・触媒・溶媒 3

HCID 167845palladium(II) acetate触媒HCID 8028Tetrahydrofuran溶媒2 回HCID 15413tert-Butyl methyl ether溶媒

反応条件

温度
0 °C

実験手順

A solution of tricyclohexylphophine (46 mg, 0.164 mmol) in tetrahydrofuran (2.5 mL) under nitrogen was charged with palladium (II) acetate (24.5mg, 0.109 mmol). The reaction mixture was stirred for 45 minutes, then cooled to 0° C. and charged with sodium tert-butoxide (270 mg, 2.73 mmol). After 5 minutes a solution of β-ethoxyacrylic acid ethyl ester (158 μL, 1.09 mmol) and 2-bromobenzyl phenyl sulfone (340 mg, 1.09 mmol) in tetrahydrofuran (2.5 mL) was added dropwise over 2 minutes. Upon complete addition the reaction was warmed to room temperature and then heated to 60° C. for 2 hours. The reaction was cooled to room temperature, then diluted with methyl tert-butyl ether (25 mL) and poured into aqueous potassium dihydrogen phosphate (0.25 M, 25 mL), pH=7. The aqueous layer was separated and saturated by addition of solid sodium chloride and extracted with ethyl acetate (2×50 mL). The organic layer was separated and washed twice with aqueous saturated sodium chloride (2×30 mL), dried over sodium sulfate, filtered and concentrated in vacuo affording 3-benzenesulfonyl-3H-indene-1-carboxylic acid ethyl ester as a light orange oil (304 mg, 0.925 mmol, 85%). 1H NMR (400 MHz, CDCl3) δ 7.88–7.86 (m, 1H), 7.75–7.72 (m, 1H), 7.49–7.43 (m, 3H), 7.36–7.32 (m, 2H), 7.27–7.25 (m, 3H), 5.15 (d, 1H, J=2.1), 4.27 (q, 2H, J=7.1), 1.34 (t, 3H, J=7.1); IR (ATR, neat) 1709, 1649, 1463, 1444, 1314, 1271, 1247, 1188, 1133, 1081, 1044, 773, 752, 722, 686, 575, 528.

後処理

  1. additionUpon complete addition the reaction
  2. temperaturewas warmed to room temperature
  3. temperatureheated to 60° C. for 2 hours
  4. temperatureThe reaction was cooled to room temperature
  5. customThe aqueous layer was separated and saturated by addition of solid sodium chloride
  6. extractionextracted with ethyl acetate (2×50 mL)
  7. customThe organic layer was separated
  8. washwashed twice with aqueous saturated sodium chloride (2×30 mL)
  9. dry with materialdried over sodium sulfate
  10. filtrationfiltered
  11. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-9aeb12b8ac724711b637d517d0227baf
出典データセット
uspto-grants-2006_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07091372B2

反応ノート

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