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3,4-Dichlorobenzyl chloride → HCID 22310865, 화합물

HRID 1072564
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HRID 1072564 반응식
[OH-].[Na+].[N+:3]([C:6]1[CH:14]=[CH:13][CH:12]=[C:11]2[C:7]=1[CH:8]=[C:9]([C:15]([O:17][CH2:18][CH3:19])=[O:16])[NH:10]2)([O-:5])=[O:4].[Cl:20][C:21]1[CH:22]=[C:23]([CH:26]=[CH:27][C:28]=1[Cl:29])[CH2:24]Cl>S([O-])(O)(=O)=O.C([N+](CCCC)(CCCC)CCCC)CCC.ClCCl>[Cl:20][C:21]1[CH:22]=[C:23]([CH:26]=[CH:27][C:28]=1[Cl:29])[CH2:24][N:10]1[C:11]2[C:7](=[C:6]([N+:3]([O-:5])=[O:4])[CH:14]=[CH:13][CH:12]=2)[CH:8]=[C:9]1[C:15]([O:17][CH2:18][CH3:19])=[O:16]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 76093,4-Dichlorobenzyl chlorideHCID 14798Sodium HydroxideHCID 283173Ethyl 4-nitro-1H-indole-2-carboxylate

생성물 1

HCID 22310865HCID 22310865, 화합물수율 78%

시약·촉매·용매 2

HCID 94433Tetrabutylammonium hydrogen sulfate촉매
HCID 6344
Dichloromethane
용매

실험 절차

Sodium hydroxide (3M, 20 ml) was added to a vigorously stirred solution of ethyl 4-nitroindole-2-carboxylate (4 g), 3,4-dichlorobenzyl chloride (4.73 ml) and tetra-n-butylammonium hydrogensulphate (0.2 g) in dichloromethane (60 ml). The reaction was stirred for 48 hours then partitioned between 2M HCl and dichloromethane. Combined organic extracts were dried (MgSO4) and concentrated in vacuo and the residue purified by column chromatography using iso-hexane: 20% ethyl acetate as eluent to give the product as a yellow crystalline solid (5.26 g, 78%); NMR δ (CD3SOCD3) 1.3 (t, 3H), 4.3 (q, 2H), 5.95 (s, 2H), 6.9 (m, 1H), 7.6 (m, 4H), 8.2 (t, 2H); M/z (+) 393.3 (M+).

후처리

  1. customthen partitioned between 2M HCl and dichloromethane
  2. dry with materialCombined organic extracts were dried (MgSO4)
  3. concentrationconcentrated in vacuo
  4. customthe residue purified by column chromatography

출처 및 근거

ORD 기록
ord-6443e55503fd46ceb9f384eb88118515
출처 데이터셋
uspto-grants-2005_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06911465B1

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