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

HRID 542856

反応式

HRID 542856 の反応式
[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

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 1049Pyridine溶媒HCID 6212Chloroform溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-ba7cb3b3a3a74618903faef23802b1b6
出典データセット
uspto-grants-1987_04
特許番号
US04659730

関連ノート

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