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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
ノート
印刷プレビュー

反応式

HRID 278194 の反応式
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]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

8

反応物 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

生成物 1

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

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

反応条件

温度
0 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-daa550378134443d9e8c1621a78b7265
出典データセット
uspto-grants-2002_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06358985B1

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート