Ethanaminium, N,N,N-triethyl-, fluoride (1:1) → HCID 16752763, 화합물

HRID 253605

반응식

HRID 253605 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([C@@H:8]([C@@H:17]2[O:22][CH2:21][CH2:20][N:19]([C:23](=[O:47])[NH:24][C@H:25]([C@H:33]([OH:46])[CH2:34][N:35](C)[C:36](OCC[Si](C)(C)C)=O)[CH2:26][CH:27]3[CH2:32][CH2:31][O:30][CH2:29][CH2:28]3)[CH2:18]2)[O:9][CH2:10][CH2:11][NH:12][C:13](=[O:16])[O:14][CH3:15])[CH:5]=[CH:6][CH:7]=1.[N+](CC)(CC)(CC)CC.[F-]>CC#N>[Cl:1][C:2]1[CH:3]=[C:4]([C@@H:8]([C@@H:17]2[O:22][CH2:21][CH2:20][N:19]([C:23](=[O:47])[NH:24][C@H:25]([C@H:33]([OH:46])[CH2:34][NH:35][CH3:36])[CH2:26][CH:27]3[CH2:32][CH2:31][O:30][CH2:29][CH2:28]3)[CH2:18]2)[O:9][CH2:10][CH2:11][NH:12][C:13](=[O:16])[O:14][CH3:15])[CH:5]=[CH:6][CH:7]=1

참가 물질

4

반응물 2

HCID 69582Ethanaminium, N,N,N-triethyl-, fluoride (1:1)HCID 66861750HCID 66861750, 화합물

생성물 1

HCID 16752763HCID 16752763, 화합물수율 12.4%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

A 10 mL flask was charged with methyl 2-((S)-(3-chlorophenyl)((R)-4-((2S,3R)-3-hydroxy-4-(N-methyl-N-(2-(trimethylsilyl)ethoxycarbonyl)amino)-1-(tetrahydro-2H-pyran-4-yl)butan-2-ylcarbamoyl)morpholin-2-yl)methoxy)ethylcarbamate (30 mg, 0.043 mmol) dissolved in MeCN (4 mL) and Et4NF (14 mg, 0.094 mmol) was added. The mixture was stirred for 0.5 h under reflux. After stirring, it was monitored by HPLC until the reaction ended. The solution was concentrated in vacuo and purified by HPLC to give the target compound (2.97 mg, 12%). 1H NMR (MeOD) 1.27-1.30 (m, 2H), 1.32-1.40 (m, 2H), 1.51-1.62 (m, 2H), 1.65-1.80 (m, 2H), 2.70 (s, 3H), 1.75-1.90 (m, 2H), 1.90-3.10 (m, 4H), 3.65 (s, 3H), 3.80-3.95 (m, 5H), 4.05-4.20 (m, 1H), 4.30 (m, 1H), 7.25-7.40 (m, 4H).

후처리

  1. temperatureunder reflux
  2. stirringAfter stirring
  3. concentrationThe solution was concentrated in vacuo
  4. custompurified by HPLC

출처 및 근거

ORD 기록
ord-30caf40a8ac34126bfc62f556e4938bb
출처 데이터셋
uspto-grants-2011_01
특허 번호
US07872028B2

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