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Phenacyl bromide → HCID 19354077, 화합물

HRID 378491
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HRID 378491 반응식
[CH2:1](Br)[C:2]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1)=[O:3].[F:11][Sb-:12]([F:17])([F:16])([F:15])([F:14])[F:13].[Na+].[CH2:19]([S:37][CH3:38])[CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][CH3:36].[Br-].[Na+]>C(C(C)=O)C>[F:11][Sb-:12]([F:17])([F:16])([F:15])([F:14])[F:13].[CH3:38][S+:37]([CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][CH3:36])[CH2:1][C:2]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1)=[O:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 6259Phenacyl bromideHCID 253881Sodium BromideHCID 5363811-(Methylsulfanyl)octadecaneHCID 16689647Sodium hexafluoroantimonate

생성물 1

HCID 19354077HCID 19354077, 화합물

시약·촉매·용매 1

HCID 6569Methyl Ethyl Ketone용매

실험 절차

In a 100 mL Erlenmeyer flask were combined 10 g (0.05 mol) phenacyl bromide, 12.93 g (0.05 mol) sodium hexafluoroantimonate, 15 g (0.05 mol) methyl octadecyl sulfide and 40 mL methyl ethyl ketone (2-butanone). The reaction mixture was heated to boiling and maintained at this temperature for 30 minutes. During this time, sodium bromide was observed to precipitate. The reaction mixture was filtered to remove the inorganic salts and the resulting solution placed on a rotary evaporator to remove solvents. The product crystallized to give the desired salt, m.p. 80-82° C. Recrystallization from isopropanol gave a very light tan salt with a melting point of 79-80° C.

후처리

  1. temperatureThe reaction mixture was heated
  2. temperaturemaintained at this temperature for 30 minutes
  3. customto precipitate
  4. filtrationThe reaction mixture was filtered
  5. customto remove the inorganic salts
  6. customthe resulting solution placed on a rotary evaporator
  7. customto remove solvents
  8. customThe product crystallized

출처 및 근거

ORD 기록
ord-4e7a78235a094b98b9fdb25f1cc51634
출처 데이터셋
uspto-grants-2000_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06031014

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