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

HRID 716554

반응식

HRID 716554 반응식
[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

참가 물질

4

반응물 2

HCID 6497Dimethyl SulfateHCID 3551932-Chloro-1,10-phenanthroline

생성물 1

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

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

반응 조건

온도
120 °C

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-22537bab64a748f98f65dfab271d7d10
출처 데이터셋
uspto-grants-2015_11
특허 번호
US09187690B2

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