Phosphorus sulfide (P2S5) → 8-Chloro-2-(2-chloroethyl)-2,3-dihydro-4-methyl-1,4-benzoxazepine-5(4H)-thione

HRID 247278

반응식

HRID 247278 반응식
[Cl:1][C:2]1[CH:17]=[CH:16][C:5]2[C:6](=O)[N:7]([CH3:14])[CH2:8][CH:9]([CH2:11][CH2:12][Cl:13])[O:10][C:4]=2[CH:3]=1.P12(SP3(SP(SP(S3)(S1)=S)(=S)S2)=S)=[S:19].[S-2].[K+].[K+]>C1(C)C=CC=CC=1>[Cl:1][C:2]1[CH:17]=[CH:16][C:5]2[C:6](=[S:19])[N:7]([CH3:14])[CH2:8][CH:9]([CH2:11][CH2:12][Cl:13])[O:10][C:4]=2[CH:3]=1

참가 물질

5

반응물 3

HCID 14817Phosphorus sulfide (P2S5)HCID 162263Potassium SulfideHCID 137262948-chloro-2-(2-chloroethyl)-2,3-dihydro-4-methyl-1,4-benzoxazepin-5(4H)one

생성물 1

HCID 137262998-Chloro-2-(2-chloroethyl)-2,3-dihydro-4-methyl-1,4-benzoxazepine-5(4H)-thione수율 73.2%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

To a solution of 43 g (0.16 mole) of 8-chloro-2-(2-chloroethyl)-2,3-dihydro-4-methyl-1,4-benzoxazepin-5(4H)-one in 400 ml of dry toluene was added a mixture of 23 g (0.12 mole) of phosphorus pentasulfide and 23 g of potassium sulfide which had been ground together. The reaction mixture was stirred and heated at reflux for 24 hr. The mixture was filtered hot and the filtrate concentrated under reduced pressure to give 25.5 g (55%) of orange oil which solidified on standing at room temperature. The solid was recrystallized from ethanol, m.p. 105°-106° C.

후처리

  1. temperatureheated
  2. temperatureat reflux for 24 hr
  3. filtrationThe mixture was filtered hot
  4. concentrationthe filtrate concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-11a7691106584167a71465ffbdf88a60
출처 데이터셋
uspto-grants-1987_11
특허 번호
US04705853

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