Dimethyl Sulfate → 9-Bromo-1-methyl-1,10-phenanthrolinium hydrogen sulfate

HRID 716558

反応式

HRID 716558 の反応式
[Br:1][C:2]1[CH:15]=[CH:14][C:13]2[C:4](=[C:5]3[C:10](=[CH:11][CH:12]=2)[CH:9]=[CH:8][CH:7]=[N:6]3)[N:3]=1.[S:16]([O:21]C)([O:19][CH3:20])(=[O:18])=[O:17]>C(OCC)C>[S:16]([O-:21])([OH:19])(=[O:18])=[O:17].[Br:1][C:2]1[CH:15]=[CH:14][C:13]2[C:4]([N:3]=1)=[C:5]1[C:10]([CH:9]=[CH:8][CH:7]=[N+:6]1[CH3:20])=[CH:11][CH:12]=2

参加物

4

反応物 2

HCID 6497Dimethyl SulfateHCID 128302472-Bromo-1,10-phenanthroline

生成物 1

HCID 866711159-Bromo-1-methyl-1,10-phenanthrolinium hydrogen sulfate収率 96.1%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

反応条件

温度
120 °C

実験手順

Under a stream of argon, to compound (7) (24.4 g; 94.2 mmol), dimethyl sulfate (77 g; 610 mmol) was added in an ice bath over 20 minutes. The reaction temperature was raised to 120° C. and the resulting reaction mixture was stirred for 1 hour. To the reaction mixture, diethyl ether was added in an ice bath, and solids which precipitated out were separated by filtration. The resulting solids were washed with a mixed solution of diethyl ether/ethanol (1/1 to 1/2) and dried under reduced pressure to give 33.6 g (yield: 96%) of the title compound (8).

後処理

  1. customthe resulting reaction mixture
  2. customsolids which precipitated out
  3. customwere separated by filtration
  4. washThe resulting solids were washed with a mixed solution of diethyl ether/ethanol (1/1 to 1/2)
  5. customdried under reduced pressure

出典と根拠

ORDレコード
ord-8536ddc0bb234c5b897bb36343c0ccdb
出典データセット
uspto-grants-2015_11
特許番号
US09187690B2

関連ノート

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