1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide → HCID 19362682、化合物

HRID 535975ノート

反応式

HRID 535975 の反応式
[C:1]([O:5][C:6]([NH:8][CH:9]([C:13]([F:16])([CH3:15])[CH3:14])[C:10](O)=[O:11])=[O:7])([CH3:4])([CH3:3])[CH3:2].Cl.CN.[CH:20]([N:23](CC)C(C)C)(C)C.O.ON1C2C=CC=CC=2N=N1.CN(C)CCCN=C=NCC>ClCCl>[F:16][C:13]([CH3:15])([CH3:14])[CH:9]([NH:8][C:6](=[O:7])[O:5][C:1]([CH3:4])([CH3:3])[CH3:2])[C:10]([NH:23][CH3:20])=[O:11]

参加物

7

反応物 5

HCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 81531DiisopropylethylamineHCID 27960291-Hydroxybenzotriazole hydrateHCID 6364545Methylamine hydrochlorideHCID 46737272DL-Valine, N-[(1,1-diMethylethoxy)carbonyl]-3-fluoro-

生成物 1

HCID 19362682HCID 19362682、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

Intermediate 66A (290 mg, 1.23 mmol) and methylamine hydrochloride (100 mg, 1.48 mmol) were dissolved in dichloromethane (5 mL) and N,N-diisopropylethylamine (0.65 mL, 3.70 mmol). 1-Hydroxybenzotriazole hydrate (283 mg, 1.85 mmol) and N-(3-dimethylaminopropyl)-N′-ethylcarbodiimide (354 mg, 1.85 mmol) were added, and the solution was stirred for 18 hours. The mixture was diluted additional dichloromethane and washed with saturated aqueous ammonium chloride solution and brine. The organic layer was separated, dried (Na2SO4), and concentrated under reduced pressure to provide intermediate 66B as an off-white solid in quantitative yield. 1H-NMR (400 MHz, (CD3)2SO) δ: 1.27 (d, 3H), 1.32 (d, 3H), 1.37 (s, 9H), 2.59 (d, 3H), 4.14 (dd, 1H), 6.72 (d, 1H), 7.93 (q, 1H).

後処理

  1. washwashed with saturated aqueous ammonium chloride solution and brine
  2. customThe organic layer was separated
  3. dry with materialdried (Na2SO4)
  4. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-17ccb678246e4d0ca8e8bccd1cffa98f
出典データセット
uspto-grants-2014_10
特許番号
US08859538B2

反応ノート

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