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Acetyl chloride → HCID 18444305、化合物

HRID 459742
ノート
印刷プレビュー

反応式

HRID 459742 の反応式
[CH3:1][N:2]([CH3:26])[C:3]1[CH:8]=[C:7]([CH2:9][N:10]([CH3:22])[CH2:11][CH2:12][C:13]2[CH:18]=[CH:17][C:16]([N+:19]([O-:21])=[O:20])=[CH:15][CH:14]=2)[C:6]([OH:23])=[C:5]([O:24][CH3:25])[CH:4]=1.C(N(C(C)C)CC)(C)C.[C:36](Cl)(=[O:38])[CH3:37]>ClCCl>[C:36]([O:23][C:6]1[C:7]([CH2:9][N:10]([CH3:22])[CH2:11][CH2:12][C:13]2[CH:18]=[CH:17][C:16]([N+:19]([O-:21])=[O:20])=[CH:15][CH:14]=2)=[CH:8][C:3]([N:2]([CH3:1])[CH3:26])=[CH:4][C:5]=1[O:24][CH3:25])(=[O:38])[CH3:37]
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 6367Acetyl chlorideHCID 81531DiisopropylethylamineHCID 9798923BN-82002

生成物 1

HCID 18444305HCID 18444305、化合物収率 60%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

0.1 g (0.278 mmol) of 4-(dimethylamino)-2-methoxy-6-({methyl[2-(4-nitrophenyl)ethyl]-amino}methyl)phenol (compound of Example 1) are placed in solution in 5 ml of anhydrous dichloromethane in the presence of 49 μl (0.42 mmol; 1.5 eq.) of diisopropylethylamine at 0° C. 30 μl (0.42 mmol; 1.5 eq.) of acetyl chloride are added dropwise to the solution and the medium is stirred for 1 hour at ambient temperature. Then 10 ml of dichloromethane is added to the reaction medium which is then washed with 3 times 10 ml of a saturated solution of sodium chloride. The organic phase is dried over magnesium sulphate, followed by filtering and concentrating under vacuum. The residue is purified on a silica column (eluent: AcOEt/Heptane: 2/1) in order to produce a yellow oil with a yield of 60%.

後処理

  1. washis then washed with 3 times 10 ml of a saturated solution of sodium chloride
  2. dry with materialThe organic phase is dried over magnesium sulphate
  3. filtrationby filtering
  4. concentrationconcentrating under vacuum
  5. customThe residue is purified on a silica column (eluent: AcOEt/Heptane: 2/1) in order
  6. customto produce a yellow oil with a yield of 60%

出典と根拠

ORDレコード
ord-d6cf385601b8464ea23ae161a71febf3
出典データセット
uspto-grants-2007_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07196084B2

反応ノート

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