Ethanaminium, N,N,N-triethyl-, fluoride (1:1) → HCID 16752763、化合物

HRID 253605

反応式

HRID 253605 の反応式
[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

参加物

4

反応物 2

HCID 69582Ethanaminium, N,N,N-triethyl-, fluoride (1:1)HCID 66861750HCID 66861750、化合物

生成物 1

HCID 16752763HCID 16752763、化合物収率 12.4%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-30caf40a8ac34126bfc62f556e4938bb
出典データセット
uspto-grants-2011_01
特許番号
US07872028B2

関連ノート

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