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1,2-Dichloroethane → N-{2-[3-(4-Cyano-3-fluoro-benzyl)-2-methyl-3H-imidazol-4-yl]-ethyl}-5-hydroxy-2-iodobenzamide

HRID 278194
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HRID 278194 반응식
Cl.Cl.[NH2:3][CH2:4][CH2:5][C:6]1[N:10]([CH2:11][C:12]2[CH:19]=[CH:18][C:15]([C:16]#[N:17])=[C:14]([F:20])[CH:13]=2)[C:9]([CH3:21])=[N:8][CH:7]=1.[OH:22][C:23]1[CH:24]=[CH:25][C:26]([I:32])=[C:27]([CH:31]=1)[C:28](O)=[O:29].O.ON1C2C=CC=CC=2N=N1.C(N(CC)CC)C.C(Cl)CCl>CN(C=O)C.O>[C:16]([C:15]1[CH:18]=[CH:19][C:12]([CH2:11][N:10]2[C:6]([CH2:5][CH2:4][NH:3][C:28](=[O:29])[C:27]3[CH:31]=[C:23]([OH:22])[CH:24]=[CH:25][C:26]=3[I:32])=[CH:7][N:8]=[C:9]2[CH3:21])=[CH:13][C:14]=1[F:20])#[N:17]
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참가 물질

8

반응물 5

HCID 111,2-DichloroethaneHCID 8471TriethylamineHCID 12380035-Hydroxy-2-iodobenzoic acidHCID 27960291-Hydroxybenzotriazole hydrateHCID 226271114-[5-(2-Amino-ethyl)-2-(methyl)-imidazol-1-ylmethyl]-2-fluoro-benzonitrile dihydrochloride

생성물 1

HCID 22627100
N-{2-[3-(4-Cyano-3-fluoro-benzyl)-2-methyl-3H-imidazol-4-yl]-ethyl}-5-hydroxy-2-iodobenzamide

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

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온도
0 °C

실험 절차

A stirred mixture of 4-[5-(2-amino-ethyl)-2-(methyl)-imidazol-1-ylmethyl]-2-fluoro-benzonitrile dihydrochloride as prepared in Example 10, Step A (2.00 g, 6.038 mmol), 5-hydroxy-2-iodobenzoic acid (1.594 g, 6.038 mmol), 1-Hydroxybenzotriazole hydrate (816 mg, 6.038 mmol), and triethylamine (2.52 mL, 18.114 mmol) in dry DMF (12.0 mL) was cooled to 0° C., and EDC (1.158 g, 6.038 mmol) was added. After stirring at 0° C. for 15 minutes, the reaction mixture was stirred at ambient temperature overnight, then poured into water and extracted with EtOAc. The organic layer was dried (MgSO4), filtered, and concentrated under reduced pressure. The residue was preabsorbed onto silica gel and purified by flash chromatography eluting with a gradient of 6-9% MeOH/CH2Cl2 to give the titled product.

후처리

  1. stirringthe reaction mixture was stirred at ambient temperature overnight
  2. extractionextracted with EtOAc
  3. dry with materialThe organic layer was dried (MgSO4)
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure
  6. customThe residue was preabsorbed onto silica gel
  7. custompurified by flash chromatography
  8. washeluting with a gradient of 6-9% MeOH/CH2Cl2

출처 및 근거

ORD 기록
ord-daa550378134443d9e8c1621a78b7265
출처 데이터셋
uspto-grants-2002_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06358985B1

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