Phosphorus sulfide (P2S5) → N-dodecylazepan-2-thione

HRID 1656893

반응식

HRID 1656893 반응식
[CH2:1]([N:13]1[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15][C:14]1=O)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH3:12].P12(SP3(SP(SP(S3)(S1)=S)(=S)S2)=S)=[S:22]>C1C=CC=CC=1>[CH2:1]([N:13]1[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15][C:14]1=[S:22])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH3:12]

참가 물질

4

반응물 2

HCID 14817Phosphorus sulfide (P2S5)HCID 42981Laurocapram

생성물 1

HCID 10108679N-dodecylazepan-2-thione수율 75.4%

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

To a solution of 5 g (17.7 mmol) of 1-n-dodecylazacycloheptan-2-one in 150 ml of benzene was added 4.18 g (9.4 mmol) of phosphorus pentasulfide and the mixture was refluxed for 1 hr. After cooling to room temperature, the mixture was filtered and the solid was washed with chloroform and ethanol. The filtrate was concentrated in vacuo and the residue was subjected to flash chromatography, (silica; (95:5)V/V hexane/ethyl acetate) to give 2.11 g (40%) of 1-n-dodecylazacycloheptane-2thione.

후처리

  1. temperaturethe mixture was refluxed for 1 hr
  2. filtrationthe mixture was filtered
  3. washthe solid was washed with chloroform and ethanol
  4. concentrationThe filtrate was concentrated in vacuo

출처 및 근거

ORD 기록
ord-62f2298416ec4fd398b32b404b3188d3
출처 데이터셋
uspto-grants-1993_10
특허 번호
US05256647

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