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Ethylenediamine → (2-Aminoethyl)[2-methyl-9-(2,4,6-trimethylphenyl)-pyridino[2,3-b]indolizin-4-yl]amine

HRID 2121584
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HRID 2121584 반응식
Cl[C:2]1[C:14]2[N:13]3[C:8]([C:9]([C:15]4[C:20]([CH3:21])=[CH:19][C:18]([CH3:22])=[CH:17][C:16]=4[CH3:23])=[CH:10][CH:11]=[CH:12]3)=[CH:7][C:6]=2[N:5]=[C:4]([CH3:24])[CH:3]=1.[CH2:25]([NH2:28])[CH2:26][NH2:27]>CN1C(=O)CCC1>[NH2:27][CH2:26][CH2:25][NH:28][C:2]1[C:14]2[N:13]3[C:8]([C:9]([C:15]4[C:20]([CH3:21])=[CH:19][C:18]([CH3:22])=[CH:17][C:16]=4[CH3:23])=[CH:10][CH:11]=[CH:12]3)=[CH:7][C:6]=2[N:5]=[C:4]([CH3:24])[CH:3]=1
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참가 물질

4

반응물 2

HCID 3301EthylenediamineHCID 69661784HCID 69661784, 화합물

생성물 1

HCID 69661982(2-Aminoethyl)[2-methyl-9-(2,4,6-trimethylphenyl)-pyridino[2,3-b]indolizin-4-yl]amine

시약·촉매·용매 1

HCID 13387N-methyl-2-pyrrolidone용매

실험 절차

Heat a solution of 4-chloro-2-methyl-9-(2,4,6-trimethylphenyl)pyridino[2,3-b]-indolizine (0.35 g, 1.04 mmol), and ethylene diamine (0.32 g, 1.04 mmol) in dry NMP (3 mL) at 100° C. for 5 h. Pour the cooled mixture onto water (30 mL) and extract twice with EtOAc (30 mL). Wash the combined extract with brine (30 mL), dry, and evaporate in vacuo. Purify by preparative TLC (20% MeOH in CH2Cl2 with 1% ammonium hydroxide) to obtain the title compound as a colorless oil.

후처리

  1. additionPour the cooled mixture onto water (30 mL)
  2. extractionextract twice with EtOAc (30 mL)
  3. washWash the
  4. extractioncombined extract with brine (30 mL)
  5. customdry
  6. customevaporate in vacuo
  7. customPurify by preparative TLC (20% MeOH in CH2Cl2 with 1% ammonium hydroxide)

출처 및 근거

ORD 기록
ord-411ada6248f04031b6986b7e1bb5cc1d
출처 데이터셋
uspto-grants-2004_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06696445B2

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