1-Bromooctane → HCID 178443887, 화합물

HRID 267181노트

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HRID 267181 반응식
[NH2:1][C:2]([NH:4][C:5]([NH2:7])=[S:6])=[S:3].[CH2:8](Br)[CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH3:15]>COCCO>[CH2:8]([SH:3]=[C:2]([NH:4][C:5]([NH2:7])=[S:6])[NH2:1])[CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH3:15]

참가 물질

4

반응물 2

HCID 81401-BromooctaneHCID 2758725Dithiobiuret

생성물 1

HCID 178443887HCID 178443887, 화합물

시약·촉매·용매 1

HCID 80192-Methoxyethanol용매

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온도
0 °C

실험 절차

The S-octyldithiobiuret was prepared as follows: To 135 g of dithiobiuret in 300 ml ethyleneglycol monomethyl ether were added 210 g of n-octyl bromide dropwise at 70°C. After 12 hours the solvent was distilled off at 12 mm. The residue was dissolved in toluene and hexane was added after which the mixture was cooled at 0°C. The solvent was decanted from the semicrystalline precipitate which was dissolved again in glacial acetic acid. The solution was poured on icewater and stirred for 2 hours. The solid was filtered, stirred with hexane in a beaker until it had completely crystallized, filtered and dried. The product had a melting point of 75°-77°C.

후처리

  1. distillationAfter 12 hours the solvent was distilled off at 12 mm
  2. dissolutionThe residue was dissolved in toluene
  3. additionhexane was added after which the mixture
  4. customThe solvent was decanted from the semicrystalline precipitate which
  5. dissolutionwas dissolved again in glacial acetic acid
  6. additionThe solution was poured on icewater
  7. filtrationThe solid was filtered
  8. stirringstirred with hexane in a beaker until it
  9. customhad completely crystallized
  10. filtrationfiltered
  11. customdried

출처 및 근거

ORD 기록
ord-53003dedb71c442da43dea05e7b5de0e
출처 데이터셋
uspto-grants-1976_03
특허 번호
US03941745

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