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Hydrochloric Acid → 2-Furan-2-ylmethyl-1-(2-methyl-cyclohexyl)-1H-benzoimidazole-5-carboxylic acid methyl ester

HRID 1750238
ノート
印刷プレビュー

反応式

HRID 1750238 の反応式
[CH3:1][O:2][C:3](=[O:27])[C:4]1[CH:9]=[CH:8][C:7]([NH:10][CH:11]2[CH2:16][CH2:15][CH2:14][CH2:13][CH:12]2[CH3:17])=[C:6]([NH:18][C:19](=O)[CH2:20][C:21]2[O:22][CH:23]=[CH:24][CH:25]=2)[CH:5]=1.Cl.O.C(=O)(O)[O-].[Na+]>O1CCOCC1>[CH3:1][O:2][C:3]([C:4]1[CH:9]=[CH:8][C:7]2[N:10]([CH:11]3[CH2:16][CH2:15][CH2:14][CH2:13][CH:12]3[CH3:17])[C:19]([CH2:20][C:21]3[O:22][CH:23]=[CH:24][CH:25]=3)=[N:18][C:6]=2[CH:5]=1)=[O:27]
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 313Hydrochloric AcidHCID 962WaterHCID 516892Sodium BicarbonateHCID 867144453-(2-Furan-2-yl-acetylamino)-4-(2-methyl-cyclohexylamino)-benzoic acid methyl ester

生成物 1

HCID 867144462-Furan-2-ylmethyl-1-(2-methyl-cyclohexyl)-1H-benzoimidazole-5-carboxylic acid methyl ester収率 93%

試薬・触媒・溶媒 1

HCID 31275
1,4-Dioxane
溶媒

実験手順

1.48 g 3-(2-Furan-2-yl-acetylamino)-4-(2-methyl-cyclohexylamino)-benzoic acid methyl ester with 15 ml of 4M hydrochloric acid in dioxane were heated in a microwave reactor to 130° C. for 15 min. Water was added to the reaction mixture and the pH was adjusted to 7 by the addition of saturated sodium bicarbonate solution. The phases were separated, and the aqueous layer was extracted with ethyl acetate twice. The combined organic layers were dried over sodium sulphate, concentrated and 1.31 g (93%) of 2-Furan-2-ylmethyl-1-(2-methyl-cyclohexyl)-1H-benzoimidazole-5-carboxylic acid methyl ester were obtained.

後処理

  1. customThe phases were separated
  2. extractionthe aqueous layer was extracted with ethyl acetate twice
  3. dry with materialThe combined organic layers were dried over sodium sulphate
  4. concentrationconcentrated

出典と根拠

ORDレコード
ord-05cb8cc9a9944122b1fbc6f10eaf3d7b
出典データセット
uspto-grants-2015_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09156796B2

反応ノート

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