1-Bromo-3-chloropropane → HCID 21438254、化合物

HRID 2397444ノート

反応式

HRID 2397444 の反応式
[Br:1][C:2]1[CH:15]=[CH:14][C:13]2[S:12][C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[NH:5][C:4]=2[CH:3]=1.C([Li])CCC.Br[CH2:22][CH2:23][CH2:24][Cl:25]>C1(C)C=CC=CC=1>[Br:1][C:2]1[CH:15]=[CH:14][C:13]2[S:12][C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[N:5]([CH2:22][CH2:23][CH2:24][Cl:25])[C:4]=2[CH:3]=1

参加物

5

反応物 3

HCID 80061-Bromo-3-chloropropaneHCID 131063502-bromo-10H-phenothiazineHCID 178418339Butyllithium

生成物 1

HCID 21438254HCID 21438254、化合物

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒3 回

実験手順

A solution of 2-bromophenothiazine (41.72 g., 0.05 mole) in 200 ml. of dry toluene was added to a stirred solution of 9.6 g. (0.15 mole) of n-butyllithium in 100 ml. of dry toluene. The stirred solution was warmed for about 2.0 hours at 45°-50° C. and then 31.5 g. (0.20 mole) of bromopropylchloride in 50 ml. of dry toluene was added. The mixture was refluxed for 15 hours. The cooled reaction mixture was washed with water, dried over sodium sulfate and the dried solution concentrated at reduced pressure. The residual oil was distilled to give the product, 2-bromo-10-(3-chloropropyl)phenothiazine.

後処理

  1. temperatureThe stirred solution was warmed for about 2.0 hours at 45°-50° C.
  2. temperatureThe mixture was refluxed for 15 hours
  3. customThe cooled reaction mixture
  4. washwas washed with water
  5. dry with materialdried over sodium sulfate
  6. concentrationthe dried solution concentrated at reduced pressure
  7. distillationThe residual oil was distilled

出典と根拠

ORDレコード
ord-7c5e8ee883c24866ada84366a0f087f3
出典データセット
uspto-grants-1977_05
特許番号
US04021552

反応ノート

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