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N,N-Dimethylglycine → HCID 86709279、化合物

HRID 517299
ノート
印刷プレビュー

反応式

HRID 517299 の反応式
Br[C:2]1[CH:7]=[CH:6][C:5]([CH2:8][N:9]2[C@@H:14]([CH3:15])[CH2:13][CH2:12][CH:11]([C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=3)[S:10]2(=[O:23])=[O:22])=[C:4]([F:24])[CH:3]=1.Cl.[N:26]1[N:27]=[CH:28][N:29]([CH:31]2[CH2:36][CH2:35][NH:34][CH2:33][CH2:32]2)[CH:30]=1.CN(C)CC(O)=O.C([O-])(=O)CC([O-])=O.C([P+](CCCC)(CCCC)CCCC)CCC.C([P+](CCCC)(CCCC)CCCC)CCC>>[F:24][C:4]1[CH:3]=[C:2]([N:34]2[CH2:33][CH2:32][CH:31]([N:29]3[CH:30]=[N:26][N:27]=[CH:28]3)[CH2:36][CH2:35]2)[CH:7]=[CH:6][C:5]=1[CH2:8][N:9]1[C@@H:14]([CH3:15])[CH2:13][CH2:12][CH:11]([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)[S:10]1(=[O:23])=[O:22]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 4

HCID 673N,N-DimethylglycineHCID 44473435Bis(tetrabutylphosphanium) propanedioateHCID 755304451609407-68-2HCID 86709280(3S)-2-(4-Bromo-2-fluorobenzyl)-3-methyl-6-phenyl-1,2-thiazinane 1,1-dioxide

生成物 1

HCID 86709279HCID 86709279、化合物収率 37%

反応条件

温度
45 °C

実験手順

A vial was charged with (3S)-2-[(4-bromo-2-fluoro-phenyl)methyl]-3-methyl-6-phenyl-thiazinane 1,1-dioxide (250 mg, 0.61 mmol), 4-(1,2,4-triazol-4-yl)piperidine hydrochloride (172 mg, 0.91 mmol), cuprous iodide (35 mg, 0.18 mmol), N,N-dimethylglycine (38 mg, 0.36 mmol) and tetrabutylphosphonium malonate (1.3 g, 1.9 mmol) and the vial was purged with nitrogen for. Dimethyl sulfoxide (3 mL) was then added and the vial was purged with nitrogen for an additional 2 minutes. The reaction mixture was then sonicated for 5 minutes and stirred at 45° C. for 20 hours. The DMSO solution was then directly purified by preparative HPLC to give (3S)-2-[[2-fluoro-4-[4-(1,2,4-triazol-4-yl)-1-piperidyl]phenyl]methyl]-3-methyl-6-phenyl-thiazinane 1,1-dioxide Stereoisomer A (109 mg, 0.23 mmol, 37% yield) as a white solid. 1H NMR (400 MHz, DMSO) δ 8.66-8.62 (s, 2H), 7.49-7.43 (m, 2H), 7.43-7.29 (m, 4H), 6.87-6.82 (m, 1H), 6.80-6.73 (m, 1H), 4.49-4.24 (m, 4H), 4.15-4.04 (m, 1H), 3.90-3.80 (m, 2H), 2.89-2.77 (m, 2H), 2.47-2.35 (m, 1H), 2.15-2.04 (m, 3H), 2.04-1.89 (m, 2H), 1.88-1.74 (m, 1H), 1.70-1.60 (m, 1H), 1.14-1.05 (d, J=6.9 Hz, 3H); LCMS [M+1]+=484.2.

後処理

  1. customthe vial was purged with nitrogen for
  2. additionDimethyl sulfoxide (3 mL) was then added
  3. customthe vial was purged with nitrogen for an additional 2 minutes
  4. customThe reaction mixture was then sonicated for 5 minutes
  5. customThe DMSO solution was then directly purified by preparative HPLC

出典と根拠

ORDレコード
ord-41347df2d4ff484087a8fce6acbb8ae9
出典データセット
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09115101B2

反応ノート

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