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Potassium Carbonate → Ethyl 3-bromo-4-[(3-methyl-2-buten-1-yl)(trifluoroacetyl)amino]-5-nitrobenzoate

HRID 852609
ノート
印刷プレビュー

反応式

HRID 852609 の反応式
[Br:1][C:2]1[CH:3]=[C:4]([CH:10]=[C:11]([N+:20]([O-:22])=[O:21])[C:12]=1[NH:13][C:14](=[O:19])[C:15]([F:18])([F:17])[F:16])[C:5]([O:7][CH2:8][CH3:9])=[O:6].C([O-])([O-])=O.[K+].[K+].Br[CH2:30][CH:31]=[C:32]([CH3:34])[CH3:33]>CC#N>[Br:1][C:2]1[CH:3]=[C:4]([CH:10]=[C:11]([N+:20]([O-:22])=[O:21])[C:12]=1[N:13]([CH2:30][CH:31]=[C:32]([CH3:34])[CH3:33])[C:14](=[O:19])[C:15]([F:17])([F:18])[F:16])[C:5]([O:7][CH2:8][CH3:9])=[O:6]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 700922-Butene, 1-bromo-3-methyl-HCID 86602878Ethyl 3-bromo-5-nitro-4-[(trifluoroacetyl)amino]benzoate

生成物 1

HCID 86602879Ethyl 3-bromo-4-[(3-methyl-2-buten-1-yl)(trifluoroacetyl)amino]-5-nitrobenzoate収率 91%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

To a solution of ethyl 3-bromo-5-nitro-4-[(trifluoroacetyl)amino]benzoate (D214) (12.0 g, 31.3 mmol, 1 equiv) in CH3CN (100 ml) was added K2CO3 (5.6 g, 40 mmol, 1.3 equiv) and 1-bromo-3-methyl-2-butene (5.1 ml, 43.8 mmol, 1.4 equiv) and the resulting mixture was refluxed for 1 h then cooled to room temperature. The precipitate formed was filtered off through a pad of celite and washed with CH3CN. The combined organic layers were concentrated in vacuo and the residue diluted with AcOEt. The organic layer was washed with brine, dried over MgSO4 and concentrated in vacuo. Purification of the residue by flash chromatography on silica gel (iso-hexane/AcOEt: 9/1 to 4/1) gave ethyl 3-bromo-4-[(3-methyl-2-buten-1-yl)(trifluoroacetyl)amino]-5-nitrobenzoate (D215) (12.9 g, 91%) as an orange oil.

後処理

  1. temperaturethe resulting mixture was refluxed for 1 h
  2. customThe precipitate formed
  3. filtrationwas filtered off through a pad of celite
  4. washwashed with CH3CN
  5. concentrationThe combined organic layers were concentrated in vacuo
  6. additionthe residue diluted with AcOEt
  7. washThe organic layer was washed with brine
  8. dry with materialdried over MgSO4
  9. concentrationconcentrated in vacuo
  10. customPurification of the residue by flash chromatography on silica gel (iso-hexane/AcOEt: 9/1 to 4/1)

出典と根拠

ORDレコード
ord-c19dcd530b5b463095d079276e551606
出典データセット
uspto-grants-2007_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07253198B2

反応ノート

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