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

HRID 1587478노트

반응식

HRID 1587478 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 40%

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

To a solution of 5g (17.7mmol) of 1-n-dodecylazacycloheptan-2-one in 150ml of benzene was added 4.18g (9.4mmol) 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.llg (40%) of 1-n-dodecylazacycloheptane-2-thione.

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-502ff0342b0a44e6b0a104d39a13916c
출처 데이터셋
uspto-grants-1993_06
특허 번호
US05218113

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