2,6-Lutidine → 1-Chloro-3-triphenylmethoxyhexane

HRID 1439112ノート

反応式

HRID 1439112 の反応式
[Cl:1][CH2:2][CH2:3][CH:4]([OH:8])[CH2:5][CH2:6][CH3:7].[C:9]1([C:15](Br)([C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)[C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1.N1C(C)=CC=CC=1C.ClC1C=CC=CC=1>O>[Cl:1][CH2:2][CH2:3][CH:4]([O:8][C:15]([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)([C:22]1[CH:23]=[CH:24][CH:25]=[CH:26][CH:27]=1)[C:16]1[CH:17]=[CH:18][CH:19]=[CH:20][CH:21]=1)[CH2:5][CH2:6][CH3:7]

参加物

6

反応物 4

HCID 79372,6-LutidineHCID 7964ChlorobenzeneHCID 11692BromotriphenylmethaneHCID 189210071-Chlorohexan-3-ol

生成物 1

HCID 203810131-Chloro-3-triphenylmethoxyhexane

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A stirred solution of 27.3 g. (0.20 moles) of 1-chloro-3-hexanol, 77.6 g. (0.24 moles) of triphenylmethyl bromide, 30.0 g. (0.28 moles of 2,6-lutidine, and 200 ml. of chlorobenzene is heated at 95° C. for 1 hour. The cooled mixture is treated with water, and the organic phase is washed successively with water and saturated sodium chloride solution. The solution is dried over magnesium sulfate and concentrated. Column chromatography of the residue on Florisil affords the subject compound as an oil, ν max. 1600, 1030, and 705 cm-1 (triphenylmethoxy group).

後処理

  1. washthe organic phase is washed successively with water and saturated sodium chloride solution
  2. dry with materialThe solution is dried over magnesium sulfate
  3. concentrationconcentrated

出典と根拠

ORDレコード
ord-260e649cd4984a8385eca55093de8e2e
出典データセット
uspto-grants-1977_11
特許番号
USRE029469

反応ノート

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