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Dichloromethane → 6-(N-methyl-N-phenylamino)hexyl chloride

HRID 344242
ノート
印刷プレビュー

反応式

HRID 344242 の反応式
[CH3:1][N:2]([CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14]O)[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C(Cl)[Cl:36]>>[CH3:1][N:2]([CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][Cl:36])[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 3

HCID 6344DichloromethaneHCID 11776TriphenylphosphineHCID 152539786-[Methyl(phenyl)amino]hexan-1-OL

生成物 1

HCID 540929106-(N-methyl-N-phenylamino)hexyl chloride

実験手順

1H-NMR (CDCl3,ppm) δ: 1.31-1.42(4 H,m), 1.51-1.63(4 H,m), 2.91(3 H,s), 3.30(2 H,t,J=7.9 Hz), 3.63(2 H,t,J=6.6 Hz), 6.64-6.70(3 H,m), 7.18-7.21(2 H,m) 6-(N-Methy-N-phenylamino)hexyl alcohol (1.1 g) and triphenylphosphine (1.3 g) were dissolved in methylene chloride (40 ml), and N-chlorosuccinylimide (0.71 g) was added, which was followed by stirring at room temperature for 1 hr 20 min. The organic layer was washed with brine, dried and the solvent was evaporated under reduced pressure. The obtained residue was purified by silica gel column chromatography to give 0.90 g of 6-(N-methy-N-phenylamino)hexyl chloride.

後処理

  1. washThe organic layer was washed with brine
  2. customdried
  3. customthe solvent was evaporated under reduced pressure
  4. customThe obtained residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-8c82d2f15b33429d87815a8abae89c22
出典データセット
uspto-grants-1999_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05864039

反応ノート

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