Phosphorus pentachloride → HCID 21315972, 화합물

HRID 614220노트

반응식

HRID 614220 반응식
[Cl:1][C:2]1[S:3][CH:4]=[C:5]2[C:11](=O)[NH:10][C:9]3[CH:13]=[CH:14][CH:15]=[CH:16][C:8]=3[O:7][C:6]=12.P(Cl)(Cl)(Cl)(Cl)[Cl:18]>C1(C)C=CC=CC=1>[Cl:1][C:2]1[S:3][CH:4]=[C:5]2[C:11]([Cl:18])=[N:10][C:9]3[CH:13]=[CH:14][CH:15]=[CH:16][C:8]=3[O:7][C:6]=12

참가 물질

4

반응물 2

HCID 24819Phosphorus pentachlorideHCID 12581868HCID 12581868, 화합물

생성물 1

HCID 21315972HCID 21315972, 화합물

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

A 4.0 g. portion of 3-chlorothieno[3,4-b][1,5]benzoxazepin-10(9H)-one (Example 12) and 4.0 g. of phosphorus pentachloride in 103 ml. of dry toluene is refluxed for 41/2 hours. The reaction temperature is concentrated, then is triturated with toluene to give 3,10-dichlorothieno[3,4-b][1,5]benzoxazepine. A 25 ml. amount of dry N-(2-hydroxyethyl)piperazine and 25 ml of dry toluene is added to the product above and the mixture is heated at 120° C. for 16 hours. The reaction mixture is concentrated to a thick oil, the oil is dissolved in hot 2N aqueous acetic acid, treated with activated charcoal and filtered through diatomaceous earth. The filtrate is cooled and precipitated with concentrated ammonium hydroxide. The precipitate is collected and extracted into methylene chloride, the organic solution is dried over anhydrous sodium sulfate and eluted through magnesium silicate with 2.5 liters of methylene chloride followed by one liter of 1:1 ethyl acetate:methylene chloride. The combined organic solvents are evaporated to yield 2.0 g. of 4-(3-chlorothieno[3,4-b][1,5]-benzoxazepin-10-yl)-1-piperazineethanol.

후처리

  1. concentrationThe reaction temperature is concentrated
  2. customis triturated with toluene

출처 및 근거

ORD 기록
ord-8112c367432b4dc09c10f93c85138da9
출처 데이터셋
uspto-grants-1979_03
특허 번호
US04144235

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