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Hydrochloric Acid → HCID 178460133、化合物

HRID 450724
ノート
印刷プレビュー

反応式

HRID 450724 の反応式
[NH2:1][C:2]1[CH:3]=[C:4]([NH:9][S:10]([C:13]2[CH:18]=[CH:17][C:16]([CH:19]([CH3:21])[CH3:20])=[CH:15][CH:14]=2)(=[O:12])=[O:11])[CH:5]=[CH:6][C:7]=1[NH2:8].Cl.[C:23]([NH:27][CH2:28][C:29](O)=O)(=[O:26])[CH2:24][CH3:25].ON1C2N=CC=CC=2N=N1.C(N=C=NCCCN(C)C)C.C(N(C(C)C)CC)(C)C>CN(C=O)C>[CH:19]([C:16]1[CH:17]=[CH:18][C:13]([S:10]([NH:9][C:4]2[CH:5]=[CH:6][C:7]3[NH:8][C:29]([CH2:28][NH:27][C:23](=[O:26])[CH2:24][CH3:25])=[N:1][C:2]=3[CH:3]=2)(=[O:12])=[O:11])=[CH:14][CH:15]=1)([CH3:21])[CH3:20]
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

8

反応物 6

HCID 313Hydrochloric AcidHCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 81531DiisopropylethylamineHCID 98681PropionylglycineHCID 181649HOAtHCID 67023917HCID 67023917、化合物

生成物 1

HCID 178460133
HCID 178460133、化合物
収率 61%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
0 °C

実験手順

To a solution of N-(3,4-diamino-phenyl)-4-isopropyl-benzenesulfonamide×HCl (500 mg, 1.32 mmol) in DMF (20 ml) at 0° C. was added propionylamino-acetic acid (170 mg, 1.32 mmol) and 1-hydroxy-7-azabenzotriazole (HOAt) (220 mg, 1.59 mmol). After stirring the mixture at 0° C. for 15 min EDC (N-ethyl-N′-(3-dimethylaminopropyl)-carbodiimide) (300 mg, 1.45 mmol) was added. DIPEA (diisopropylethylamine) (0.92 ml, 5.29 mmol) was added after stirring another 15 min at 0° C. The mixture was stirred at room temperature for 16 h, and then concentrated under reduced pressure. The residue was partitioned between ethyl acetate and saturated aqueous NaHCO3 and the organic layer was dried over MgSO4, filtered, and the solvent evaporated under reduced pressure. A solution of the obtained oil in acetic acid was heated to 70° C. for 6 h. After evaporation of the solvent in vacuo the residue was purified by column chromatography to give the product as a yellow oil (320 mg, 61%).

後処理

  1. additionwas added
  2. stirringThe mixture was stirred at room temperature for 16 h
  3. concentrationconcentrated under reduced pressure
  4. customThe residue was partitioned between ethyl acetate and saturated aqueous NaHCO3
  5. dry with materialthe organic layer was dried over MgSO4
  6. filtrationfiltered
  7. customthe solvent evaporated under reduced pressure
  8. temperatureA solution of the obtained oil in acetic acid was heated to 70° C. for 6 h
  9. customAfter evaporation of the solvent in vacuo the residue
  10. customwas purified by column chromatography

出典と根拠

ORDレコード
ord-8d9ad607050c481cb04f0423e2542194
出典データセット
uspto-grants-2013_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08486984B2

反応ノート

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