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Methyl iodide → HCID 86746472、化合物

HRID 1646127
ノート
印刷プレビュー

反応式

HRID 1646127 の反応式
[CH:1]([N-]C(C)C)(C)[CH3:2].[Li+].[C:9]([O-:14])(=[O:13])[CH2:10][CH:11]=C.[CH2:15]([C:19]1[N:20]([CH2:36][C:37]2[CH:42]=[CH:41][CH:40]=[CH:39][C:38]=2[Cl:43])[C:21](/[CH:24]=[C:25](\[CH2:30][C:31]2[S:32][CH:33]=[CH:34][CH:35]=2)/C(OC)=O)=[CH:22][N:23]=1)[CH2:16][CH2:17][CH3:18].CI>O1CCCC1.[Cl-].[NH4+]>[CH2:15]([C:19]1[N:20]([CH2:36][C:37]2[CH:42]=[CH:41][CH:40]=[CH:39][C:38]=2[Cl:43])[C:21](/[CH:24]=[C:25](\[CH2:30][C:31]2[S:32][CH:33]=[CH:34][CH:35]=2)/[CH:10]([CH3:11])[C:9]([O:14][CH2:1][CH3:2])=[O:13])=[CH:22][N:23]=1)[CH2:16][CH2:17][CH3:18]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 6328Methyl iodideHCID 2724682Lithium diisopropylamideHCID 69710893-Butenoic acid, ion(1-)HCID 11743343methyl (E) 3-[2-n-butyl-1-[(2-chlorophenyl)methyl]-1H-imidazol-5-yl]-(2-thienyl)methyl-2-propenoate

生成物 1

HCID 86746472HCID 86746472、化合物

試薬・触媒・溶媒 2

HCID 8028
Tetrahydrofuran
溶媒
HCID 25517Ammonium Chloride溶媒

実験手順

Lithium diisopropylamide (0.85 mmol, 1M in tetrahydrofuran) is cooled to -78° under argon and a solution of ethyl (E)-4-[2-n-butyl-1-[(2-chlorophenyl)methyl}-1H-imidazol-5-yl]-3-(2-thienyl)methyl)-3-butenoate (0.709 mmol), prepared as in Example 13 using methyl (E) 3-[2-n-butyl-1-[(2-chlorophenyl)methyl]-1H-imidazol-5-yl]-(2-thienyl)methyl-2-propenoate (Example 1), in tetrahydrofuran (5 mL) is added. After 10 minutes methyl iodide (0.71 mmol) is added. The mixture is then stirred at room temperature overnight, diluted with 10% ammonium chloride and extracted with ethyl acetate. The dried, concentrated product is chromatographed over silica gel with 6:4 hexanes/ethyl acetate to give the title compound. (ii) (E)-1-[2-n-butyl-1-{(2-chlorophenyl)methyl}-1H-imidazol-5-yl]-3-methyl-3-(1H-tetrazol-5-yl)-2-(2-thienyl)methyl-1-propene

後処理

  1. extractionextracted with ethyl acetate
  2. customThe dried, concentrated product is chromatographed over silica gel with 6:4 hexanes/ethyl acetate

出典と根拠

ORDレコード
ord-fbba6d66799241c2a00ba2cacd584a36
出典データセット
uspto-grants-1993_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05177096

反応ノート

読み込み中…

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