1,2,3,4-Tetrahydro-1-naphthalenol → 1-Chloro-1,2,3,4-tetrahydronaphthalene

HRID 542856

반응식

HRID 542856 반응식
[CH:1]1(O)[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH2:4][CH2:3][CH2:2]1.S(Cl)([Cl:14])=O>C(Cl)(Cl)Cl.N1C=CC=CC=1>[Cl:14][CH:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH2:4][CH2:3][CH2:2]1

참가 물질

5

반응물 2

HCID 107231,2,3,4-Tetrahydro-1-naphthalenolHCID 24386Thionyl Chloride

생성물 1

HCID 1887171-Chloro-1,2,3,4-tetrahydronaphthalene

시약·촉매·용매 2

HCID 1049Pyridine용매HCID 6212Chloroform용매

실험 절차

One hundred grams of 1,2,3,4-tetrahydro-1-naphthol were dissolved in 1 liter of chloroform and 53.9 ml of pyridine. The mixture was cooled with an external ice bath and 98.6 ml of thionyl chloride were added over a 1 hour period. The reaction mixture was stirred an additional 2 hours with cooling, concentrated in vacuo, and the residue taken up in 1 liter of methylene chloride. The methylene chloride solution was washed with water, a 5% sodium bicarbonate solution, water again, dried over sodium sulfate, and evaporated to dryness to provide the desired intermediate 1,2,3,4-tetrahydro-1-chloronaphthalene.

후처리

  1. temperatureThe mixture was cooled with an external ice bath
  2. temperaturewith cooling
  3. concentrationconcentrated in vacuo
  4. washThe methylene chloride solution was washed with water
  5. dry with materiala 5% sodium bicarbonate solution, water again, dried over sodium sulfate
  6. customevaporated to dryness

출처 및 근거

ORD 기록
ord-ba7cb3b3a3a74618903faef23802b1b6
출처 데이터셋
uspto-grants-1987_04
특허 번호
US04659730

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