1-Bromo-3-chloropropane → HCID 21438254, 화합물

HRID 2397444노트

반응식

HRID 2397444 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 21438254HCID 21438254, 화합물

시약·촉매·용매 1

HCID 1140Toluene용매3회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-7c5e8ee883c24866ada84366a0f087f3
출처 데이터셋
uspto-grants-1977_05
특허 번호
US04021552

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