Iodoethane → 3-ethyl-1,1,2-trimethyl-1H-benzo[e]indol-3-ium iodide

HRID 2186039

반응식

HRID 2186039 반응식
[CH2:1]([I:3])[CH3:2].[CH3:4][C:5]1([CH3:19])[C:13]2[C:12]3[CH:14]=[CH:15][CH:16]=[CH:17][C:11]=3[CH:10]=[CH:9][C:8]=2[N:7]=[C:6]1[CH3:18]>C(#N)C>[I-:3].[CH3:4][C:5]1([CH3:19])[C:13]2[C:12]3[CH:14]=[CH:15][CH:16]=[CH:17][C:11]=3[CH:10]=[CH:9][C:8]=2[N+:7]([CH2:1][CH3:2])=[C:6]1[CH3:18]

참가 물질

4

반응물 2

HCID 6340IodoethaneHCID 1705302,3,3-Trimethylbenzoindolenine

생성물 1

HCID 100902153-ethyl-1,1,2-trimethyl-1H-benzo[e]indol-3-ium iodide수율 91.3%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

Ethyl iodide (1.1 g, 7.2 mmol) was added to an acetonitrile solution (40 ml) of 1,1,2-trimethylbenz[e]indole (1) (1.0 g, 4.8 mmol, Daiichi Pure Chemicals Co., Ltd.), and then the mixture was heated under reflux for 2 days. The reaction mixture was concentrated under reduced pressure, and ether (80 ml) was added to the residue. The resulting solid was repeatedly washed with ether to obtain the title compound (2) as a dark violet solid (1.6 g, 91%). mp. 213-218° C. (decomposition).

후처리

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 2 days
  3. concentrationThe reaction mixture was concentrated under reduced pressure, and ether (80 ml)
  4. additionwas added to the residue
  5. washThe resulting solid was repeatedly washed with ether

출처 및 근거

ORD 기록
ord-9d9cbc1d84c94af69f860275d98eabac
출처 데이터셋
uspto-grants-2002_06
특허 번호
US06403625B1

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