1-Hydroxybenzotriazole → HCID 86714415、化合物

HRID 1750203ノート

反応式

HRID 1750203 の反応式
[O:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[CH2:6][C:7]([OH:9])=O.C1C=CC2N(O)N=NC=2C=1.CCN(C(C)C)C(C)C.[CH3:29][O:30][C:31](=[O:45])[C:32]1[CH:37]=[CH:36][C:35]([NH:38][CH:39]([CH2:42][CH3:43])[CH2:40][CH3:41])=[C:34]([NH2:44])[CH:33]=1>CN(C=O)C.O.C(Cl)CCl>[CH3:29][O:30][C:31](=[O:45])[C:32]1[CH:37]=[CH:36][C:35]([NH:38][CH:39]([CH2:40][CH3:41])[CH2:42][CH3:43])=[C:34]([NH:44][C:7](=[O:9])[CH2:6][C:2]2[O:1][CH:5]=[CH:4][CH:3]=2)[CH:33]=1

参加物

8

反応物 4

HCID 757711-HydroxybenzotriazoleHCID 75974Furan-2-acetic acidHCID 81531Diisopropylethylamine2 回HCID 61311526Methyl 3-amino-4-(pentan-3-ylamino)benzoate

生成物 1

HCID 86714415HCID 86714415、化合物収率 87%

試薬・触媒・溶媒 3

HCID 111,2-Dichloroethane溶媒HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

To a solution of 4.48 g of 2-furylacetic acid in 30 ml of dry DMF 1.00 g of HOBT, 3.97 g of EDC and 1.8 ml of DIPEA were added at 0° C. After 30 min 3.50 g of 3-amino-4-(1-ethyl-propylamino)-benzoic acid methyl ester and 1.8 ml of DIPEA were added and the reaction was stirred at it for 16 h. The reaction was then poured into water and extracted with ethyl acetate three times. The combined organic phases were washed with saturated aqueous sodium carbonate solution and saturated aqueous ammonium chloride solution, dried over magnesium sulphate and concentrated to obtain 4.44 g (87%) of 4-(1-Ethyl-propylamino)-3-(2-furan-2-yl-acetylamino)-benzoic acid methyl ester.

後処理

  1. extractionextracted with ethyl acetate three times
  2. washThe combined organic phases were washed with saturated aqueous sodium carbonate solution and saturated aqueous ammonium chloride solution
  3. dry with materialdried over magnesium sulphate
  4. concentrationconcentrated

出典と根拠

ORDレコード
ord-c5b41ad70ccd4455b9fef9362a942927
出典データセット
uspto-grants-2015_10
特許番号
US09156796B2

反応ノート

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