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Triethylamine → HCID 86658429、化合物

HRID 1968879
ノート
印刷プレビュー

反応式

HRID 1968879 の反応式
[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[C@@H:7]1[CH2:9][C@H:8]1[C:10]([OH:12])=O.C(Cl)(=O)C(Cl)=O.[Si:19]([O:26][C:27]1[CH:32]=[CH:31][C:30]([NH:33][CH2:34][C@@H:35]([NH:40][C:41](=[O:47])[O:42][C:43]([CH3:46])([CH3:45])[CH3:44])[C@@H:36]([CH3:39])[CH2:37][CH3:38])=[CH:29][CH:28]=1)([C:22]([CH3:25])([CH3:24])[CH3:23])([CH3:21])[CH3:20].C(N(CC)CC)C>CN(C=O)C.C(OCC)C.ClCCl>[Si:19]([O:26][C:27]1[CH:32]=[CH:31][C:30]([N:33]([CH2:34][C@@H:35]([NH:40][C:41](=[O:47])[O:42][C:43]([CH3:44])([CH3:46])[CH3:45])[C@@H:36]([CH3:39])[CH2:37][CH3:38])[C:10]([C@@H:8]2[CH2:9][C@H:7]2[C:2]2[CH:3]=[CH:4][CH:5]=[CH:6][N:1]=2)=[O:12])=[CH:29][CH:28]=1)([C:22]([CH3:23])([CH3:24])[CH3:25])([CH3:21])[CH3:20]
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

8

反応物 4

HCID 8471TriethylamineHCID 65578Oxalyl chlorideHCID 39235822rac-(1R,2R)-2-(pyridin-2-yl)cyclopropane-1-carboxylic acidHCID 67114485HCID 67114485、化合物

生成物 1

HCID 86658429HCID 86658429、化合物収率 77%

試薬・触媒・溶媒 3

HCID 6228
Dimethylformamide
触媒
HCID 3283Diethyl Ether溶媒
HCID 6344Dichloromethane溶媒

反応条件

温度
35 °C

実験手順

A solution of trans-2-pyridin-2-yl-cyclopropylcarboxylic acid (270 mg, 1.7 mmol) and dichloromethane (15 mL) was treated with oxalyl chloride (170 μL, 2.0 mmol) and DMF (1 drop). The resulting reaction mixture was maintained at 35° C. for 3 h, then concentrated under reduced pressure to dryness. The residue was dissolved in dichloromethane (15 mL), and treated with tert-butyl (2S,3S)-1-(4-(tert-butyldimethylsilyloxy)phenylamino)-3-methylpentan-2-ylcarbamate (700 mg, 1.7 mmol) and triethylamine (690 μL, 5.0 mmol). The reaction mixture was maintained at room temperature overnight, then diluted with diethyl ether (30 mL) washed with saturated aqueous sodium bicarbonate (30 mL) and brine (30 mL), then dried over MgSO4, filtered and concentrated to afford a residue that was purified by column chromatography on silica gel (eluting with 15% ethyl acetate in hexanes) to afford tert-butyl (2S,3S)-1-(N-(4-(tert-butyldimethylsilyloxy)phenyl)-trans-2-(pyridin-2-yl)cyclopropanecarboxamido)-3-methylpentan-2-ylcarbamate (720 mg, 77% yield) as a yellow oil: 1H NMR (400 MHz, CDCl3) δ 8.04-8.13 (m, 1H), 7.25-7.36 (m, 1H), 6.91-7.00 (m, 1H), 6.87-6.91 (m, 1H), 6.76-6.86 (m, 2H), 6.55-6.62 (m, 1H), 6.46-6.55 (m, 1H), 4.83-4.98 (m, 1H), 4.15-4.27 (m, 1H), 3.45-3.64 (m, 1H), 2.81-2.93 (m, 1H), 2.23-2.48 (m, 1H), 1.68-1.81 (m, 1H), 1.37 (s, 3H), 1.29-1.52 (m, 2H), 1.28 (s, 3H), 1.25 (s, 3H), 1.15-1.22 (m, 1H), 0.86-0.97 (m, 1H), 0.78 (d, J=5.1 Hz, 9H), 0.67-0.71 (m, 3H), 0.60-0.67 (m, 3H), −0.06-0.02 (m, 6H); LRMS (ESI) m/e 568.3 [(M+H)+, calcd for C32H50N3O4Si 568.3].

後処理

  1. customThe resulting reaction mixture
  2. concentrationconcentrated under reduced pressure to dryness
  3. dissolutionThe residue was dissolved in dichloromethane (15 mL)
  4. temperatureThe reaction mixture was maintained at room temperature overnight
  5. washwashed with saturated aqueous sodium bicarbonate (30 mL) and brine (30 mL)
  6. dry with materialdried over MgSO4
  7. filtrationfiltered
  8. concentrationconcentrated
  9. customto afford a residue that
  10. customwas purified by column chromatography on silica gel (eluting with 15% ethyl acetate in hexanes)

出典と根拠

ORDレコード
ord-0c4d1bd6ef6a4990b11f161f7e1d3d5c
出典データセット
uspto-grants-2013_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08426414B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート