Cesium carbonate → Methyl 5-(tert-butoxycarbonylamino)-1-methylcyclohex-3-enecarboxylate

HRID 74997ノート

反応式

HRID 74997 の反応式
[CH3:1][C:2]12[CH2:17][CH:6]([N:7]([C:10]([O:12][C:13]([CH3:16])([CH3:15])[CH3:14])=[O:11])[C:8]1=[O:9])[CH:5]=[CH:4][CH2:3]2.IC1C2CC(C)(C(=O)N2[C:27](OC(C)(C)C)=[O:28])CC=1.C(=O)([O-])[O-].[Cs+].[Cs+]>CO>[C:13]([O:12][C:10]([NH:7][CH:6]1[CH2:17][C:2]([CH3:1])([C:8]([O:28][CH3:27])=[O:9])[CH2:3][CH:4]=[CH:5]1)=[O:11])([CH3:16])([CH3:15])[CH3:14]

参加物

5

反応物 3

HCID 10796Cesium carbonateHCID 68008024Tert-butyl 1-methyl-7-oxo-6-azabicyclo[3.2.1]oct-3-ene-6-carboxylateHCID 86667435Tert butyl 4-iodo-1-methyl-7-oxo-6-azabicyclo[3.2.1]oct-3-ene-6-carboxylate

生成物 1

HCID 67285544Methyl 5-(tert-butoxycarbonylamino)-1-methylcyclohex-3-enecarboxylate

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a solution of tert-butyl 1-methyl-7-oxo-6-azabicyclo[3.2.1]oct-3-ene-6-carboxylate, 52e, (4.93 g, 20.78 mmol) in MeOH (100 mL) was added cesium carbonate (13.54 g, 41.56 mmol). The reaction was stirred overnight and then concentrated in vacuo. The cesium salts were precipitated with Et2O and filtered. The ether filtrate was evaporated to give 5.5 g of a yellow oil that was used without further purification.

後処理

  1. concentrationconcentrated in vacuo
  2. customThe cesium salts were precipitated with Et2O
  3. filtrationfiltered
  4. customThe ether filtrate was evaporated

出典と根拠

ORDレコード
ord-b4c8293e3e304bb4a76cf91d58d46185
出典データセット
uspto-grants-2014_09
特許番号
US08829007B2

反応ノート

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