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

HRID 716554

反応式

HRID 716554 の反応式
[Cl: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].[Cl: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 3551932-Chloro-1,10-phenanthroline

生成物 1

HCID 866711149-Chloro-1-methyl-1,10-phenanthrolinium hydrogen sulfate収率 78%

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 (3) (5.2 g; 24.2 mmol), dimethyl sulfate (22.1 g; 175 mmol) was added at room temperature over 10 minutes. The reaction temperature was raised to 120° C. and the resulting reaction mixture was stirred for 1 hour and then cooled to room temperature. Diethyl ether was added thereto and light brown crude crystals which precipitated out were separated by filtration. The obtained crude crystals were washed with a solution of diethyl ether/ethanol=1/1 to 1/2 and dried under reduced pressure to give 6.17 g of the title compound (4).

後処理

  1. customthe resulting reaction mixture
  2. temperaturecooled to room temperature
  3. customlight brown crude crystals which precipitated out
  4. customwere separated by filtration
  5. customThe obtained crude crystals
  6. washwere washed with a solution of diethyl ether/ethanol=1/1 to 1/2
  7. customdried under reduced pressure

出典と根拠

ORDレコード
ord-22537bab64a748f98f65dfab271d7d10
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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