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Triethylamine → (1S,2S)-N-((R)-2-Hydroxy-1-(4-((S)-2-methylbutoxy)phenyl)ethyl)-2-(thiophen-2-yl)cyclopropanecarboxamide

HRID 454974
ノート
印刷プレビュー

反応式

HRID 454974 の反応式
Cl.[OH:2][CH2:3][C@H:4]([NH-:17])[C:5]1[CH:10]=[CH:9][C:8]([O:11][CH2:12][C@@H:13]([CH3:16])[CH2:14][CH3:15])=[CH:7][CH:6]=1.C(N(CC)CC)C.[S:25]1[CH:29]=[CH:28][CH:27]=[C:26]1[C@H:30]1[CH2:32][C@@H:31]1[C:33](Cl)=[O:34]>ClCCl>[OH:2][CH2:3][C@H:4]([NH:17][C:33]([C@H:31]1[CH2:32][C@@H:30]1[C:26]1[S:25][CH:29]=[CH:28][CH:27]=1)=[O:34])[C:5]1[CH:10]=[CH:9][C:8]([O:11][CH2:12][C@@H:13]([CH3:16])[CH2:14][CH3:15])=[CH:7][CH:6]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 8471TriethylamineHCID 86658144(1S,2S)-2-thiophen-2-yl-cyclopropanecarboxylic chlorideHCID 86658145{(R)-2-hydroxy-1-[4-((S)-2-methyl-butoxy)-phenyl]-ethyl}-amide HCl

生成物 1

HCID 51348369(1S,2S)-N-((R)-2-Hydroxy-1-(4-((S)-2-methylbutoxy)phenyl)ethyl)-2-(thiophen-2-yl)cyclopropanecarboxamide収率 58%

試薬・触媒・溶媒 1

HCID 6344
Dichloromethane
溶媒
2 回

実験手順

To a solution of (1S,2S)-2-Thiophen-2-yl-cyclopropanecarboxylic acid (1.08 g, 6.45 mmol) in dichloromethane (50 ml) in an ice-bath was added oxalyl chloride (6.50 ml, 64.4 mmol), then DMF (0.1 ml) under nitrogen. The reaction mixture was stirred for 30 minutes at 0° C. The excessive solvent was removed on ratovapor and dried under high vacuum for 2 hrs to give (1S,2S)-2-thiophen-2-yl-cyclopropanecarboxylic chloride. In a separated 250 ml round-bottom flask was charged with {(R)-2-hydroxy-1-[4-((S)-2-methyl-butoxy)-phenyl]-ethyl}-amide HCl (6.47 mmol), dichloromethane (60 ml) and triethylamine (4.30 ml, 32.35 mmol) in an ice cold bath under nitrogen. The (1S,2S)-2-Thiophen-2-yl-cyclopropanecarboxylic chloride, made freshly in dichloromethane (10 ml) was added into the reaction mixture dropwise. The final reaction mixture was stirred for 1.5 hrs at room temperature. The finished reaction was quenched with water. The organic phase was washed with brine (3×30 ml), dried over MgSO4, filtrated, concentrated in vacuum and purified via column chromatography on silica gel with a gradient of 0%-100% of ethyl acetate in hexane to give a white solid (1.42 g, 58% yield): 1H NMR (400 MHz, CHLOROFORM-d) δ ppm 7.25 (d, J=8.6 Hz, 2H), 7.09 (m, 1H), 6.91 (m, 3H), 6.82 (d, J=3.5 Hz, 1H), 6.23 (d, J=6.1 Hz, 1H), 5.06 (td, J=6.3, 4.3 Hz, 1H), 3.91 (m, 2H), 3.78 (m, 2H), 2.75 (m, 2H), 1.88 (m, 1H), 1.70 (m, 2H), 1.58 (m, 1H), 1.29 (m, 2H), 1.03 (d, J=6.8 Hz, 3H), 0.96 (t, J=7.5 Hz, 3H); LCMS (ESI) m/e 374.2 [(M+H)+, calcd for C21H28NO3S 374.5].

後処理

  1. additionwas added into the reaction mixture dropwise
  2. customThe final reaction mixture
  3. customThe finished reaction
  4. customwas quenched with water
  5. washThe organic phase was washed with brine (3×30 ml)
  6. dry with materialdried over MgSO4
  7. filtrationfiltrated
  8. concentrationconcentrated in vacuum
  9. custompurified via column chromatography on silica gel with a gradient of 0%-100% of ethyl acetate in hexane

出典と根拠

ORDレコード
ord-4dc8064f76094c189d28fd5e95a9dbf2
出典データセット
uspto-grants-2013_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08497271B2

反応ノート

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