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1-Chloro-4-(chloromethyl)benzene → HCID 11654892、化合物

HRID 1988836
ノート
印刷プレビュー

反応式

HRID 1988836 の反応式
[F:1][C:2]1[CH:20]=[CH:19][C:5]([CH2:6][O:7][C:8]2[CH:13]=[CH:12][N:11]=[C:10]3[C:14]([CH3:18])=[C:15]([CH3:17])[NH:16][C:9]=23)=[CH:4][CH:3]=1.CC(C)([O-])C.[K+].C1OCCOCCOCCOCCOCCOC1.[Cl:45][C:46]1[CH:53]=[CH:52][C:49]([CH2:50]Cl)=[CH:48][CH:47]=1>O1CCCC1>[ClH:45].[Cl:45][C:46]1[CH:53]=[CH:52][C:49]([CH2:50][N:16]2[C:9]3[C:10](=[N:11][CH:12]=[CH:13][C:8]=3[O:7][CH2:6][C:5]3[CH:19]=[CH:20][C:2]([F:1])=[CH:3][CH:4]=3)[C:14]([CH3:18])=[C:15]2[CH3:17])=[CH:48][CH:47]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 77231-Chloro-4-(chloromethyl)benzeneHCID 2855718-Crown-6HCID 23665647Potassium tert-butoxideHCID 687053187-[(4-Fluorophenyl)methoxy]-2,3-dimethyl-1H-pyrrolo[3,2-b]pyridine

生成物 1

HCID 11654892HCID 11654892、化合物収率 20%

試薬・触媒・溶媒 1

HCID 8028
Tetrahydrofuran
溶媒

実験手順

7-(4-fluorobenzyloxy)-2,3-dimethyl-1H-pyrrolo[3,2-b]pyridine (25 mg, 0.105 mmol) prepared in Step 1, potassium tert-butoxide (13.6 mg, 0.163 mmol), and a catalytic amount of 18-crown-6 were added to anhydrous tetrahydrofuran (2 ml). 4-Chlorobenzyl chloride (0.089 ml, 0.160 mmol) was added to the reaction mixture, which was then stirred for 12 hours at room temperature. The reaction mixture was concentrated under reduced pressure. The resulting residue was purified with silica gel column chromatography (ethyl acetate/methylene chloride/methanol=10/10/1, (v/v/v)), dissolved in ethyl acetate (1 ml), and then saturated with hydrochloric acid gas. The resulting precipitate was filtered to give the titled compound as a white solid (6.9 mg, 15.8%).

後処理

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. customThe resulting residue was purified with silica gel column chromatography (ethyl acetate/methylene chloride/methanol=10/10/1, (v/v/v))
  3. dissolutiondissolved in ethyl acetate (1 ml)
  4. filtrationThe resulting precipitate was filtered

出典と根拠

ORDレコード
ord-e78ad4a6295c4e9f8689bcd88ec3213a
出典データセット
uspto-grants-2010_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07642269B2

反応ノート

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