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Phenacyl bromide → HCID 19354077、化合物

HRID 378491
ノート
印刷プレビュー

反応式

HRID 378491 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

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

生成物 1

HCID 19354077HCID 19354077、化合物

試薬・触媒・溶媒 1

HCID 6569Methyl Ethyl Ketone溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-4e7a78235a094b98b9fdb25f1cc51634
出典データセット
uspto-grants-2000_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06031014

反応ノート

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