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2,6-Dichlorobenzoic acid → (+/-)-2,6-Dichloro-N-[[1-(dimethylamino)cyclopentyl] (phenyl)methyl]benzamide

HRID 20829
ノート
印刷プレビュー

反応式

HRID 20829 の反応式
[Cl:1][C:2]1[CH:10]=[CH:9][CH:8]=[C:7]([Cl:11])[C:3]=1[C:4]([OH:6])=O.ON1C2C=CC=CC=2N=N1.C1(N=C=NC2CCCCC2)CCCCC1.[NH2:37][CH:38]([C:47]1[CH:52]=[CH:51][CH:50]=[CH:49][CH:48]=1)[C:39]1([N:44]([CH3:46])[CH3:45])[CH2:43][CH2:42][CH2:41][CH2:40]1.C(N(C(C)C)CC)(C)C.C(O)C(N)(CO)CO>C(Cl)Cl.CN1CCCC1=O>[Cl:11][C:7]1[CH:8]=[CH:9][CH:10]=[C:2]([Cl:1])[C:3]=1[C:4]([NH:37][CH:38]([C:39]1([N:44]([CH3:46])[CH3:45])[CH2:43][CH2:42][CH2:41][CH2:40]1)[C:47]1[CH:52]=[CH:51][CH:50]=[CH:49][CH:48]=1)=[O:6]
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 6

HCID 57582,6-Dichlorobenzoic acidHCID 6503Tris(hydroxymethyl)aminomethaneHCID 10868DicyclohexylcarbodiimideHCID 757711-HydroxybenzotriazoleHCID 81531DiisopropylethylamineHCID 11521393{1-[Amino(phenyl)methyl]cyclopentyl}dimethylamine

生成物 1

HCID 11632528
(+/-)-2,6-Dichloro-N-[[1-(dimethylamino)cyclopentyl] (phenyl)methyl]benzamide
収率 83.2%

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 13387N-methyl-2-pyrrolidone溶媒

実験手順

To a solution of 2,6-dichlorobenzoic acid (20 mg; 0.105 mmol) in DCM (2 ml) and N-methylpyrrolidinone (0.1-0.5 ml) was added 1-hydroxybenzotriazole (18 mg; 0.11 mmol) and PL-dicyclohexylcarbodiimide (88 mg; 0.14 mmol; Polymer Labs 1.59 mmol/g). The mixture was shaken at room temperature for 1 hour and then 1-[amino(phenyl)methyl]cyclopentyl}dimethylamine dihydrochloride D2 (20 mg; 0.07 mmol) and PS-diisopropylethylamine (82 mg; 0.21 mmol; Polymer Labs 2.59 mmol/g) were then added and shaking continued overnight at room temperature. An excess of PS-Trisamine was then added and after shaking for a further 4 h, the mixture was filtered and the resins washed well with DCM and methanol. The filtrate was reduced in volume by evaporation in vacuo and loaded onto an SCX cartridge (500 mg). Washing with DCM, then methanol followed by elution with 1M ammonia in methanol afforded the title product (22.8 mg). 1H NMR (CDCl3) δ: 0.98 (1H, m), 1.26 (1H, m), 1.40 (2H, m), 1.68 (2H, m), 1.85 (2H, m), 2.22 (6H, s), 5.08 (1H, bs), 7.27 (7H, m), and 7.47 (2H, m). Mass Spectrum (Electrospray LC/MS): Found 391 (MH+). C21H2435Cl2N2O requires 390. Ret. time 1.88 min.

後処理

  1. additionwere then added
  2. stirringshaking
  3. waitcontinued overnight at room temperature
  4. stirringafter shaking for a further 4 h
  5. filtrationthe mixture was filtered
  6. washthe resins washed well with DCM and methanol
  7. customThe filtrate was reduced in volume by evaporation in vacuo
  8. washWashing with DCM
  9. washmethanol followed by elution with 1M ammonia in methanol

出典と根拠

ORDレコード
ord-574184220f5b41b0b8bb23e5553139f4
出典データセット
uspto-grants-2010_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07745642B2

反応ノート

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