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Triethylamine → methyl 2-(4-phenylbenzyloxy)-6,7-dihydro-5H-benzocycloheptene-8-carboxylate

HRID 1169325
ノート
印刷プレビュー

反応式

HRID 1169325 の反応式
[C:1]1([C:7]2[CH:30]=[CH:29][C:10]([CH2:11][O:12][C:13]3[CH:28]=[CH:27][C:16]4[CH2:17][CH2:18][CH2:19][CH:20]([C:23]([O:25][CH3:26])=[O:24])[C:21](=O)[C:15]=4[CH:14]=3)=[CH:9][CH:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[BH4-].[Na+].C(N(CC)CC)C.CS(Cl)(=O)=O.C1CCN2C(=NCCC2)CC1>ClCCl.CO.O>[C:1]1([C:7]2[CH:8]=[CH:9][C:10]([CH2:11][O:12][C:13]3[CH:28]=[CH:27][C:16]4[CH2:17][CH2:18][CH2:19][C:20]([C:23]([O:25][CH3:26])=[O:24])=[CH:21][C:15]=4[CH:14]=3)=[CH:29][CH:30]=2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=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

9

反応物 5

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 811841,8-Diazabicyclo(5.4.0)undec-7-eneHCID 4311764Sodium borohydrideHCID 22989966methyl 3-(4-phenylbenzyloxy)-5-oxo-6,7,8,9-tetrahydro-5H-benzocycloheptene-6-carboxylate

生成物 1

HCID 22990066
methyl 2-(4-phenylbenzyloxy)-6,7-dihydro-5H-benzocycloheptene-8-carboxylate
収率 59.1%

試薬・触媒・溶媒 3

HCID 887Methanol溶媒HCID 962Water溶媒HCID 6344Dichloromethane溶媒

反応条件

温度
-40 °C

実験手順

To methyl 3-(4-phenylbenzyloxy)-5-oxo-6,7,8,9-tetrahydro-5H-benzocycloheptene-6-carboxylate (2.31 g, 5.77 mmol) dissolved in a mixed solvent of dichloromethane (50 ml) and methanol (15 ml) was added at −40° C. (inner temperature) sodium borohydride (327 mg, 8.64 mmol), and the resulting mixture was stirred at −20° C. to −10° C. for 2 hours. The reaction mixture was cooled to −40° C., was mixed with water (20 ml) and extracted with dichloromethane (50 ml, 10 ml×2). The combined organic layers were dried with anhydrous magnesium sulfate and were then concentrated under reduced pressure. To the residue dissolved in dichloromethane (40 ml) were added at 0° C. triethylamine (4.02 ml, 28.8 mmol) and methanesulfonyl chloride (0.67 ml, 8.7 mmol), and the resulting mixture was stirred at room temperature for 16 hours. In order to complete the reaction, DBU (2.59 ml, 17.3 mmol) was added, and the resulting mixture was stirred at room temperature for 12 hours. The reaction mixture was concentrated under reduced pressure, was mixed with water (30 ml) and was extracted with ethyl acetate (40 ml, 15 ml×2). The combined organic layers were washed with 1 N hydrochloric acid (5 ml×3), were dried with anhydrous magnesium sulfate and were then concentrated under reduced pressure, and the residue was subjected to column chromatography (silica gel: 60 g, toluene). The objective fractions were concentrated under reduced pressure and the residue was mixed with ethyl acetate and diisopropyl ether, and an insoluble material was collected by filtration. The insoluble material was washed with diisopropyl ether and was then dried under reduced pressure to obtain methyl 2-(4-phenylbenzyloxy)-6,7-dihydro-5H-benzocycloheptene-8-carboxylate (1.31 g, 3.41 mmol, 59%).

後処理

  1. extractionextracted with dichloromethane (50 ml, 10 ml×2)
  2. dry with materialThe combined organic layers were dried with anhydrous magnesium sulfate
  3. concentrationwere then concentrated under reduced pressure
  4. dissolutionTo the residue dissolved in dichloromethane (40 ml)
  5. stirringthe resulting mixture was stirred at room temperature for 16 hours
  6. additionwas added
  7. stirringthe resulting mixture was stirred at room temperature for 12 hours
  8. concentrationThe reaction mixture was concentrated under reduced pressure
  9. additionwas mixed with water (30 ml)
  10. extractionwas extracted with ethyl acetate (40 ml, 15 ml×2)
  11. washThe combined organic layers were washed with 1 N hydrochloric acid (5 ml×3)
  12. dry with materialwere dried with anhydrous magnesium sulfate
  13. concentrationwere then concentrated under reduced pressure
  14. concentrationThe objective fractions were concentrated under reduced pressure
  15. additionthe residue was mixed with ethyl acetate and diisopropyl ether
  16. filtrationan insoluble material was collected by filtration
  17. washThe insoluble material was washed with diisopropyl ether
  18. customwas then dried under reduced pressure

出典と根拠

ORDレコード
ord-66eb600b7741478ab15ad589953435f4
出典データセット
uspto-grants-2003_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06627651B1

反応ノート

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