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Methyl iodide → Methyl hexyldithiocarbamate

HRID 2412784
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HRID 2412784 반응식
[CH2:1]([NH2:7])[CH2:2][CH2:3][CH2:4][CH2:5][CH3:6].[OH-].[Na+].[C:10](=[S:12])=[S:11].[CH3:13]I>O>[CH2:1]([NH:7][C:10](=[S:12])[S:11][CH3:13])[CH2:2][CH2:3][CH2:4][CH2:5][CH3:6]
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참가 물질

6

반응물 4

HCID 6328Methyl iodideHCID 6348Carbon DisulfideHCID 8102HexylamineHCID 14798Sodium Hydroxide

생성물 1

HCID 15917037Methyl hexyldithiocarbamate수율 89.3%

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

Water (500 ml.) was added to hexylamine (490.0 g.) and a solution of sodium hydroxide (193.6 g.) in water (700 ml.) was added thereto under ice-cooling and stirring. Carbon disulfide (367.8 g.) was added dropwise thereto over 2 hours at 2° to 10° C. and then methyl iodide (687.3 g.) was added dropwise thereto over 1 hour at 0° to 5° C. The resulting mixture was stirred for 30 minutes at the same temperature and for 2 hours at ambient temperature. The reaction mixture was extracted with diethyl ether (1.5 l.). The extract was washed with a saturated aqueous solution of sodium chloride (300 ml.), dried over magnesium sulfate and concentrated to give an oil of methyl N-hexyldithiocarbamate (825.5 g.).

후처리

  1. temperatureunder ice-cooling
  2. waitover 1 hour at 0° to 5° C
  3. stirringThe resulting mixture was stirred for 30 minutes at the same temperature and for 2 hours at ambient temperature
  4. extractionThe reaction mixture was extracted with diethyl ether (1.5 l.)
  5. washThe extract was washed with a saturated aqueous solution of sodium chloride (300 ml.)
  6. dry with materialdried over magnesium sulfate
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-02f5ac0e4e01499384397468307030a8
출처 데이터셋
uspto-grants-1985_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04493833

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