Ethyl Acetate → 3-[(R)-2,2,1-trimethylpropylamino]-4-(2-hydroxy-4-cyanophenyl)amino-3-cyclobutene-1,2-dione

HRID 357291ノート

反応式

HRID 357291 の反応式
C(O[C:4]1[C:5](=[O:19])[C:6](=[O:18])[C:7]=1[NH:8][C:9]1[CH:14]=[CH:13][C:12]([C:15]#[N:16])=[CH:11][C:10]=1[OH:17])C.[CH3:20][C:21]([CH3:26])([CH3:25])[C@H:22]([NH2:24])[CH3:23].C(OCC)(=O)C>CCCCCC>[CH3:20][C:21]([CH3:26])([CH3:25])[C@H:22]([NH:24][C:4]1[C:5](=[O:19])[C:6](=[O:18])[C:7]=1[NH:8][C:9]1[CH:14]=[CH:13][C:12]([C:15]#[N:16])=[CH:11][C:10]=1[OH:17])[CH3:23]

参加物

5

反応物 3

HCID 8857Ethyl AcetateHCID 5324845(R)-3,3-Dimethyl-2-aminobutaneHCID 105153373-Ethoxy-4-(2-hydroxy-4-cyanoanilino)-3-cyclobutene-1,2-dione

生成物 1

HCID 442723363-[(R)-2,2,1-trimethylpropylamino]-4-(2-hydroxy-4-cyanophenyl)amino-3-cyclobutene-1,2-dione

試薬・触媒・溶媒 1

HCID 8058Hexane溶媒

実験手順

A mixture of 3-ethoxy-4-(2-hydroxy-4-cyanophenyl)amino-3-cyclobutene-1,2-dione (0.395 g, 0.0015 mol) and (R)-2,2,1-trimethylpropylamine (0.2M in ethanol, 23 ml, 0.0046 mol) was stirred at room temperature for two days. TLC (2:1 ethyl acetate:hexane) indicates a loss of starting material. The ethanol is evaporated on a rotary evaporator. The reaction is taken up in ethyl acetate and extracted well with 0.25N HCl. The organic layer is washed once with distilled water, dried (Na2SO4), and evaporated to a solid. The solid is collected and washed with diethyl ether to give 3-[(R)-2,2,1-trimethylpropylamino]-4-(2-hydroxy-4-cyanophenyl)amino-3-cyclobutene-1,2-dione, 0.345 g (0.00095 mol, 72%).

後処理

  1. customThe ethanol is evaporated on a rotary evaporator
  2. extractionextracted well with 0.25N HCl
  3. washThe organic layer is washed once with distilled water
  4. dry with materialdried (Na2SO4)
  5. customevaporated to a solid
  6. customThe solid is collected
  7. washwashed with diethyl ether

出典と根拠

ORDレコード
ord-1382cf94d94b492d9eb0919e3544fdda
出典データセット
uspto-grants-1998_11
特許番号
US05840764

反応ノート

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