Phosphorus sulfide (P2S5) → 2-(2-Chloroethyl)-2,3-dihydro-4-methylnaphth[2,3-f][1,4]oxazepine-5(4H)-thione

HRID 4806

반응식

HRID 4806 반응식
[Cl:1][CH2:2][CH2:3][CH:4]1[CH2:10][N:9]([CH3:11])[C:8](=O)[C:7]2[CH:13]=[C:14]3[C:19](=[CH:20][C:6]=2[O:5]1)[CH:18]=[CH:17][CH:16]=[CH:15]3.P12(SP3(SP(SP(S3)(S1)=S)(=S)S2)=S)=[S:22].[S-2].[K+].[K+]>C1(C)C=CC=CC=1>[Cl:1][CH2:2][CH2:3][CH:4]1[CH2:10][N:9]([CH3:11])[C:8](=[S:22])[C:7]2[CH:13]=[C:14]3[C:19](=[CH:20][C:6]=2[O:5]1)[CH:18]=[CH:17][CH:16]=[CH:15]3

참가 물질

5

반응물 3

HCID 14817Phosphorus sulfide (P2S5)HCID 162263Potassium SulfideHCID 137263632-(2-chloroethyl)-2,3-dihydro-4-methylnaphth[2,3-f][1,4]oxazepin-5(4H)-one

생성물 1

HCID 137263642-(2-Chloroethyl)-2,3-dihydro-4-methylnaphth[2,3-f][1,4]oxazepine-5(4H)-thione

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

To a solution of 16.6 g (0.06 mole) of 2-(2-chloroethyl)-2,3-dihydro-4-methylnaphth[2,3-f][1,4]oxazepin-5(4H)-one in 150 ml of dry toluene was added a mixture of 8.6 g (0.045 mole) of phosphorus pentasulfide and 8.6 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. Yellow solid, 6.5 g (35%) was obtained which was recrystallized from ethanol, m.p. 166°-168° C.

후처리

  1. temperatureheated
  2. temperatureat reflux for 24 hr
  3. filtrationThe mixture was filtered hot
  4. concentrationthe filtrate concentrated under reduced pressure
  5. customYellow solid, 6.5 g (35%) was obtained which
  6. customwas recrystallized from ethanol, m.p. 166°-168° C.

출처 및 근거

ORD 기록
ord-b8c658f123854d16ae3bbcb4846c2600
출처 데이터셋
uspto-grants-1988_02
특허 번호
US04727152

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