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1,1'-Carbonyldiimidazole → HCID 19068519、化合物

HRID 1957777
ノート
印刷プレビュー

反応式

HRID 1957777 の反応式
[C:1]([NH:4][CH:5]([CH2:9][C:10]([C:12]1[CH:17]=[C:16]([Cl:18])[CH:15]=[CH:14][C:13]=1[NH2:19])=[O:11])[C:6]([OH:8])=O)(=[O:3])[CH3:2].C(N1C=CN=C1)(N1C=CN=C1)=O.[NH2:32][C@H:33]([C:36]1[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=1)[CH2:34][OH:35]>CN(C=O)C>[C:1]([NH:4][CH:5]([CH2:9][C:10]([C:12]1[CH:17]=[C:16]([Cl:18])[CH:15]=[CH:14][C:13]=1[NH2:19])=[O:11])[C:6]([NH:32][CH:33]([C:36]1[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=1)[CH2:34][OH:35])=[O:8])(=[O:3])[CH3:2]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 682631,1'-CarbonyldiimidazoleHCID 2724025(R)-beta-aminophenethyl alcoholHCID 10755519HCID 10755519、化合物

生成物 1

HCID 19068519HCID 19068519、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

反応条件

温度
5 °C

実験手順

To a stirred solution of 2-acetamido-4-(2-amino-5-chlorophenyl)-4-oxo-butyric acid (0.569 g; 2 mmol) in dry DMF (8 ml), 1,1'-carbonyldiimidazole (0.34 g; 2.1 mmol) was added portionwise at 5°-8° C. under nitrogen. After stirring at 5° C. for 1.5 h, (R)-(-)-2-amino-2-phenylethanol (0.33 g; 2.4 mmol) in dry DMF (6 ml) was added dropwise at 3°-5° C. The reaction was then stirred for 2 h in an ice bath and 16 h at room temperature, quenched with water and extracted with ethyl acetate. The organic layer was washed with water, dried with an. sodium sulfate and concentrated to dryness. The residue was purified by flash-chromatography on silica gel (ethyl acetate:methanol=98:2) to yield 2-acetylamino-4-(2-amino-5-chlorophenyl)-N-(2-hydroxy-1-phenyl-ethyl)-4-oxobutyramide as a yellow solid (0.18 g; 22%; m.p. 212°-215° C.) (pure diastereoisomer with Rf<).

後処理

  1. stirringThe reaction was then stirred for 2 h in an ice bath and 16 h at room temperature
  2. customquenched with water
  3. extractionextracted with ethyl acetate
  4. washThe organic layer was washed with water
  5. customdried with an
  6. concentrationsodium sulfate and concentrated to dryness
  7. customThe residue was purified by flash-chromatography on silica gel (ethyl acetate:methanol=98:2)

出典と根拠

ORDレコード
ord-b2ade4a69b63473ca2d9cafd1622f01b
出典データセット
uspto-grants-1998_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05786508

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート