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Triethylamine → HCID 71581630, 화합물

HRID 530251
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HRID 530251 반응식
[CH2:1]1[C:10]2[C:5](=[CH:6][C:7]([C@@:11]([C@@H:14]3[C@@H:19]([CH3:20])[CH2:18][CH2:17][CH2:16][C:15]3([CH3:22])[CH3:21])([OH:13])[CH3:12])=[CH:8][CH:9]=2)[CH2:4][CH2:3][NH:2]1.C(N(CC)CC)C.[N:30]([Si](C)(C)C)=[C:31]=[O:32]>ClCCl>[OH:13][C@@:11]([C:7]1[CH:6]=[C:5]2[C:10](=[CH:9][CH:8]=1)[CH2:1][N:2]([C:31]([NH2:30])=[O:32])[CH2:3][CH2:4]2)([C@@H:14]1[C@@H:19]([CH3:20])[CH2:18][CH2:17][CH2:16][C:15]1([CH3:21])[CH3:22])[CH3:12]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 70696Trimethylsilyl isocyanateHCID 117720122HCID 117720122, 화합물

생성물 1

HCID 71581630HCID 71581630, 화합물수율 43.5%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

To a solution of compound of the crude product of Example 13c (28 mg, 0.1 mmol) in dichloromethane (2 mL) was added triethylamine (55 mg, 0.5 mmol) and isocyanatotrimethylsilane (47 mg, 0.4 mmol). The reaction was stirred at room temperature overnight. The mixture was diluted with dichloromethane and washed with water, saturated aqueous ammonium chloride, saturated aqueous sodium bicarbonate and brine. The organic phase was dried over anhydrous sodium sulfate and concentrated under reduced pressure to afford the title compound as a yellow oil (15 mg). Mass spectrum (LC ESI +ve) m/z 345 (M+H+).

후처리

  1. washwashed with water, saturated aqueous ammonium chloride, saturated aqueous sodium bicarbonate and brine
  2. dry with materialThe organic phase was dried over anhydrous sodium sulfate
  3. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-108cee94b1854724ab95c7e8b994177b
출처 데이터셋
uspto-grants-2016_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09353063B2

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