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Diethyl Ether → HCID 57517330、化合物

HRID 1629717
ノート
印刷プレビュー

反応式

HRID 1629717 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]([NH2:11])([CH3:10])[CH3:9])=[CH:4][C:3]=1[CH3:12].CC(C)([O-])C.[K+].[I:19][C:20]1[CH:25]=[CH:24][CH:23]=[C:22](I)[CH:21]=1.CCOCC>COCCOC>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]([NH:11][C:22]2[CH:23]=[CH:24][CH:25]=[C:20]([I:19])[CH:21]=2)([CH3:9])[CH3:10])=[CH:4][C:3]=1[CH3:12]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 3283Diethyl EtherHCID 12270Benzene, 1,3-diiodo-HCID 23665647Potassium tert-butoxideHCID 57517329HCID 57517329、化合物

生成物 1

HCID 57517330HCID 57517330、化合物

試薬・触媒・溶媒 1

HCID 80711,2-Dimethoxyethane溶媒

実験手順

A suspension of amine INT 22 (2.8 g, 15.24 mmol) and potassium tert-butoxide (5.99 g, 53.4 mmol) in DME (25 mL) was purged with argon for 5 minutes. Then, PEPPSI-IPr® (207 mg, 0.305 mmol) and 1,3-diiodobenzene (5.03 g, 15.24 mmol) were added and the flask was closed. The mixture was stirred at room temperature over the weekend. The crude reaction mixture was treated with Et2O (50 mL) and filtered. The residue was washed with more Et2O (30 mL) and the combined filtrates were concentrated. The crude was purified by chromatography on silica gel (cyclohexane/CH2Cl2).

後処理

  1. customwas purged with argon for 5 minutes
  2. customthe flask was closed
  3. customThe crude reaction mixture
  4. filtrationfiltered
  5. washThe residue was washed with more Et2O (30 mL)
  6. concentrationthe combined filtrates were concentrated
  7. customThe crude was purified by chromatography on silica gel (cyclohexane/CH2Cl2)

出典と根拠

ORDレコード
ord-a98f5baf998e49f097c9e9daff46fdf8
出典データセット
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08791100B2

反応ノート

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