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Cesium carbonate → Methyl-3-(1,4-dioxa-8-azaspiro[4.5]dec-8-yl)benzoate

HRID 1051982
ノート
印刷プレビュー

反応式

HRID 1051982 の反応式
CC(C1C=C(C(C)C)C(C2C=CC=CC=2P(C2CCCCC2)C2CCCCC2)=C(C(C)C)C=1)C.C(=O)([O-])[O-].[Cs+].[Cs+].[CH2:41]1[O:50][C:44]2([CH2:49][CH2:48][NH:47][CH2:46][CH2:45]2)[O:43][CH2:42]1.[CH3:51][O:52][C:53](=[O:61])[C:54]1[CH:59]=[CH:58][CH:57]=[C:56](Br)[CH:55]=1>C1(C)C=CC=CC=1.C([O-])(=O)C.[Pd+2].C([O-])(=O)C.CC(O)(C)C>[CH3:51][O:52][C:53](=[O:61])[C:54]1[CH:59]=[CH:58][CH:57]=[C:56]([N:47]2[CH2:48][CH2:49][C:44]3([O:50][CH2:41][CH2:42][O:43]3)[CH2:45][CH2:46]2)[CH:55]=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

8

反応物 4

HCID 10796Cesium carbonateHCID 12070Methyl 3-bromobenzoateHCID 674351,4-Dioxa-8-azaspiro(4.5)decaneHCID 111557942-Dicyclohexylphosphino-2',4',6'-triisoprophylbiphenyl

生成物 1

HCID 60059302Methyl-3-(1,4-dioxa-8-azaspiro[4.5]dec-8-yl)benzoate

試薬・触媒・溶媒 3

HCID 167845
palladium(II) acetate
触媒
HCID 1140Toluene溶媒2 回
HCID 6386tert-Butanol溶媒2 回

反応条件

温度
120 °C

実験手順

Procedure adopted from Tetrahedron Lett., 2007, 48, 2519. A thick-walled glass reaction vessel was charged with palladium(II)acetate (235 mg, 1.05 mmol), X-Phos (500 mg, 1.05 mmol, 2-dicyclohexylphosphino-2′,4′,6′-triisopropylbiphenyl), cesium carbonate (6.82 g, 20.95 mmol) and 5:1 (v/v) toluene:t-BuOH (20 mL). The stirred contents were purged with nitrogen and a solution of 4-piperidone ethylene ketal (2.70 mL, 20.95 mmol) and methyl-3-bromobenzoate (4.95 g, 23.02 mmol) in 5:1 (v/v) toluene:t-BuOH (100 mL) was added. After stirring for 2 minutes, the vessel was sealed and the reaction mixture was heated at 120° C. for 16 hours. Upon cooling to room temperature, the reaction mixture was filtered through celite and the filtrate was concentrated.

後処理

  1. customA thick-walled glass reaction vessel
  2. customThe stirred contents were purged with nitrogen
  3. customthe vessel was sealed
  4. temperatureUpon cooling to room temperature
  5. filtrationthe reaction mixture was filtered through celite
  6. concentrationthe filtrate was concentrated

出典と根拠

ORDレコード
ord-d3973b10688b4c2a97a5e2ce273c5f9b
出典データセット
uspto-grants-2016_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09388176B2

反応ノート

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