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Cesium carbonate → HCID 66756714、化合物

HRID 1642631
ノート
印刷プレビュー

反応式

HRID 1642631 の反応式
C(O[C:4](=O)[CH2:5][C:6]1[CH:11]=[CH:10][C:9]([N+:12]([O-:14])=[O:13])=[C:8]([O:15][CH2:16][C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[CH:7]=1)C.[CH2:24]([O:31][C:32]1[CH:39]=[CH:38][CH:37]=C(F)[C:33]=1[C:34]#[N:35])[C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1.C([O-])([O-])=O.[Cs+].[Cs+]>CN(C=O)C.CCOC(C)=O>[CH2:24]([O:31][C:32]1[CH:39]=[CH:38][CH:37]=[C:4]([CH2:5][C:6]2[CH:11]=[CH:10][C:9]([N+:12]([O-:14])=[O:13])=[C:8]([O:15][CH2:16][C:17]3[CH:18]=[CH:19][CH:20]=[CH:21][CH:22]=3)[CH:7]=2)[C:33]=1[C:34]#[N:35])[C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=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

6

反応物 3

HCID 10796Cesium carbonateHCID 30234822-Benzyloxy-6-fluorobenzonitrileHCID 66757012HCID 66757012、化合物

生成物 1

HCID 66756714HCID 66756714、化合物

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒2 回HCID 8857Ethyl Acetate溶媒

反応条件

温度
80 °C

実験手順

(3-Benzyloxy-4-nitrophenyl)-acetic acid ethyl ester (Step C) (1.90 g, 6.03 mmol) and 2-benzyloxy-6-fluorobenzonitrile (Step D) (2.74 g, 12.1 mmol) are dissolved in DMF (18 mL) and added dropwise to a suspension of Cs2CO3 (5.89 g, 18.1 mmol) in DMF (18 mL). The mixture is heated to 80° C. for 1.5 h, then stirred at 60° C. for 16 h. The mixture is diluted with EtOAc (350 mL) and extracted with 1N HCl (2×75 mL), followed by brine (75 mL). The organic phase is dried over Na2SO4 and concentrated. The residue is taken up in THF (18 mL), MeOH (18 mL) and 1N NaOH (36 mL). Decarboxylation is complete after 2 h, the reaction mixture is poured into ice water (100 mL) and acidified to pH ˜2 with 6N HCl. The mixture is extracted with EtOAc (2×200 mL) and the organic phase is washed with brine (75 mL), dried over Na2SO4 and concentrated to afford a brown oil. Purification by flash column (10-75% EtOAc/hexanes) affords 2-benzyloxy-6-(3-benzyloxy-4-nitrobenzyl)-benzonitrile as an off-white solid: MS (M+H)+=451.

後処理

  1. extractionextracted with 1N HCl (2×75 mL)
  2. dry with materialThe organic phase is dried over Na2SO4
  3. concentrationconcentrated
  4. waitDecarboxylation is complete after 2 h
  5. additionthe reaction mixture is poured into ice water (100 mL)
  6. extractionThe mixture is extracted with EtOAc (2×200 mL)
  7. washthe organic phase is washed with brine (75 mL)
  8. dry with materialdried over Na2SO4
  9. concentrationconcentrated
  10. customto afford a brown oil
  11. customPurification by flash column (10-75% EtOAc/hexanes)

出典と根拠

ORDレコード
ord-00bf8f5ff598478faba2a154eb9d0b80
出典データセット
uspto-grants-2012_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08119666B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート