Carbon Disulfide → Antimony N-(2-octyl)-N-ethyldithiocarbamate

HRID 1288403

반응식

HRID 1288403 반응식
[CH3:1][CH:2]([NH:9][CH2:10][CH3:11])[CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH3:8].O=[Sb:13]O[Sb]=O.CCCCCC.[C:23](=[S:25])=[S:24]>O>[CH3:1][CH:2]([N:9]([CH2:10][CH3:11])[C:23](=[S:24])[S-:25])[CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH3:8].[Sb+3:13].[CH3:1][CH:2]([N:9]([CH2:10][CH3:11])[C:23](=[S:24])[S-:25])[CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH3:8].[CH3:1][CH:2]([N:9]([CH2:10][CH3:11])[C:23](=[S:24])[S-:25])[CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH3:8]

참가 물질

6

반응물 4

HCID 6348Carbon DisulfideHCID 8058HexaneHCID 27652Oxo(oxostibanyloxy)stibaneHCID 5250531-Heptanamine, 1-methyl, N-ethyl

생성물 1

HCID 21501793Antimony N-(2-octyl)-N-ethyldithiocarbamate

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
68 °C

실험 절차

In a 3-liter, three-neck, round-bottom flask equipped with a stirrer, thermometer, dropping funnel and condenser was placed 157 g. (grams) (1.0 mole) of N-(2-octyl)-N-ethylamine, 49 g. (0.168 mole) of antimony trioxide and 1000 ml. (milliliters) of hexane. The stirred mixture was heated to reflux (68°C.) and 80 g. (1.05 moles) of carbon disulfide was added over a period of 1 hour. The mixture was stirred at reflux for an additional 3 hours, and then the water generated during the reaction was azeotroped off (9 ml.). The mixture was filtered hot in order to remove any unreacted antimony oxide. The hexane solution was cooled to room temperature and the hexane was then removed at reduced pressure. A viscous oil was isolated having an Index of refraction ND22 =1.627.

후처리

  1. customIn a 3-liter, three-neck, round-bottom flask equipped with a stirrer
  2. temperatureThe stirred mixture was heated
  3. temperatureat reflux for an additional 3 hours
  4. customwas azeotroped off (9 ml.)
  5. filtrationThe mixture was filtered hot in order
  6. customto remove any unreacted antimony oxide
  7. temperatureThe hexane solution was cooled to room temperature
  8. customthe hexane was then removed at reduced pressure
  9. customA viscous oil was isolated

출처 및 근거

ORD 기록
ord-ee4a5f3811d6448da4ab0885712207dd
출처 데이터셋
uspto-grants-1976_10
특허 번호
US03988249

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