1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide → HCID 19362682, 화합물

HRID 2110237노트

반응식

HRID 2110237 반응식
[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]

참가 물질

7

반응물 5

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

생성물 1

HCID 19362682HCID 19362682, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-8f76440738e748bfaf63ed0d3be3f501
출처 데이터셋
uspto-grants-2009_04
특허 번호
US07517874B2

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