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Carbon tetrabromide → HCID 59455124、化合物

HRID 1401674
ノート
印刷プレビュー

反応式

HRID 1401674 の反応式
[CH2:1]([C:4]1[CH:11]=[CH:10][C:7]([CH:8]=O)=[CH:6][N:5]=1)[CH2:2][CH3:3].[C:12](Br)(Br)([Br:14])[Br:13].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>C(Cl)Cl>[Br:13][C:12]([Br:14])=[CH:8][C:7]1[CH:10]=[CH:11][C:4]([CH2:1][CH2:2][CH3:3])=[N:5][CH:6]=1
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 11205Carbon tetrabromideHCID 11776TriphenylphosphineHCID 450798906-Propylpyridine-3-carbaldehyde

生成物 1

HCID 59455124HCID 59455124、化合物収率 12.2%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

6-Propylnicotinaldehyde (0.2 g, 0.00134 mol) was dissolved in DCM (4 mL). Carbon tetrabromide (0.887 g, 0.00268 mol) and triphenylphosphine (1.4 g, 0.00536 mol) were added to the solution followed by stirring at RT overnight. After insoluble matter was removed by filtration, the filtrate was concentrated under reduced pressure. The residue was purified through column chromatography (3% ethylacetate:hexane in silica 100-200 mesh, diameter of column—5.0 cm, height of silica—approx. 5 inch) to provide the desired compound as a yellow colored oil (0.05 g).

このページの内容参加物実験手順後処理出典と根拠反応ノート

後処理

  1. customAfter insoluble matter was removed by filtration
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. customThe residue was purified through column chromatography (3% ethylacetate:hexane in silica 100-200 mesh, diameter of column—5.0 cm, height of silica—approx. 5 inch)

出典と根拠

ORDレコード
ord-1c5754b1a52145e3861e6be6f99725ca
出典データセット
uspto-grants-2014_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08907097B2

反応ノート

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