Iodine → 1-[(3,4-Dihydro-2-naphthalenyl)methyl]-4-anilino isonipecotamide

HRID 2072471노트

반응식

HRID 2072471 반응식
[NH:1]([C:8]1([C:14]([NH2:16])=[O:15])[CH2:13][CH2:12][NH:11][CH2:10][CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Cl[CH2:18][C:19]1[CH2:28][CH2:27][C:26]2[C:21](=[CH:22][CH:23]=[CH:24][CH:25]=2)[CH:20]=1.C(=O)([O-])[O-].[Na+].[Na+].II>C1(C)C=CC=CC=1.C(Cl)Cl>[CH:20]1[C:21]2[C:26](=[CH:25][CH:24]=[CH:23][CH:22]=2)[CH2:27][CH2:28][C:19]=1[CH2:18][N:11]1[CH2:10][CH2:9][C:8]([NH:1][C:2]2[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=2)([C:14]([NH2:16])=[O:15])[CH2:13][CH2:12]1

참가 물질

7

반응물 4

HCID 807IodineHCID 10340Sodium CarbonateHCID 964284-Anilinopiperidine-4-carboxamideHCID 127714333-(Chloromethyl)-1,2-dihydronaphthalene

생성물 1

HCID 214082231-[(3,4-Dihydro-2-naphthalenyl)methyl]-4-anilino isonipecotamide

시약·촉매·용매 2

HCID 1140Toluene용매HCID 6344Dichloromethane용매

실험 절차

A mixture of 4-anilino isonipecotamide (5.5 g), 3,4-dihydro-2-chloromethylnaphthalene (4.0 g), and powdered sodium carbonate (3.5 g) in toluene (200 ml) containing several crystals of iodine is refluxed for 14 hours with vigorous stirring under nitrogen. The reaction mixture is then cooled, diluted with methylene chloride (100 ml), and filtered. The filtrate is concentrated and the crude product triturated with ethyl acetate (100 ml) to give the title compound.

후처리

  1. temperatureis refluxed for 14 hours
  2. temperatureThe reaction mixture is then cooled
  3. filtrationfiltered
  4. concentrationThe filtrate is concentrated
  5. customthe crude product triturated with ethyl acetate (100 ml)

출처 및 근거

ORD 기록
ord-489e56ecdefa4457972d39fdb2be6887
출처 데이터셋
uspto-grants-1977_09
특허 번호
US04051248

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