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Diethylamine → Cyclopentyl(2S)-5-(4-bromophenyl)-2-[(tert-butoxycarbonyl)amino]pent-4-ynoate

HRID 425030
ノート
印刷プレビュー

反応式

HRID 425030 の反応式
[C:1]([O:5][C:6]([NH:8][C@@H:9]([CH2:18][C:19]#[CH:20])[C:10]([O:12][CH:13]1[CH2:17][CH2:16][CH2:15][CH2:14]1)=[O:11])=[O:7])([CH3:4])([CH3:3])[CH3:2].I[C:22]1[CH:27]=[CH:26][C:25]([Br:28])=[CH:24][CH:23]=1.C(NCC)C>C(OCC)C.[Cu](I)I.Cl[Pd](Cl)([P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)[P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1>[Br:28][C:25]1[CH:26]=[CH:27][C:22]([C:20]#[C:19][CH2:18][C@H:9]([NH:8][C:6]([O:5][C:1]([CH3:4])([CH3:3])[CH3:2])=[O:7])[C:10]([O:12][CH:13]2[CH2:14][CH2:15][CH2:16][CH2:17]2)=[O:11])=[CH:23][CH:24]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 3

HCID 8021DiethylamineHCID 115221-Bromo-4-iodobenzeneHCID 59243606cyclopentyl(2S)-2-[(tert-butoxycarbonyl)amino]pent-4-ynoate

生成物 1

HCID 59243578Cyclopentyl(2S)-5-(4-bromophenyl)-2-[(tert-butoxycarbonyl)amino]pent-4-ynoate収率 75%

試薬・触媒・溶媒 3

HCID 83717Copper iodide触媒
HCID 178418476
HCID 178418476、化合物
触媒
HCID 3283Diethyl Ether溶媒

実験手順

To a mixture of cyclopentyl(2S)-2-[(tert-butoxycarbonyl)amino]pent-4-ynoate (2.45 g, 8.72 mmol) and 4-iodo-bromobenzene (2.96 g, 10.46 mmol) in diethyl ether (4 ml) was added copper iodide (0.166 g, 0.872 mmol) and PdCl2(PPh3)2 (0.306 g, 0.436 mmol). Diethylamine (5.43 ml, 52.3 mmol) was then added and the mixture stirred at RT. After 2 hrs, LCMS showed complete reaction. The mixture was poured onto water and extracted with diethyl ether. The combined organic layers were washed with water and brine, dried over magnesium sulphate, filtered and evaporated in vacuo. The crude residue was subjected to column chromatography eluting with 5 to 10% EtOAc in hexanes. Yield=2.9 g, 6.51 mmol, 75% yield. LCMS purity 98%: m/z 437 [M+H]+.

後処理

  1. customreaction
  2. additionThe mixture was poured onto water
  3. extractionextracted with diethyl ether
  4. washThe combined organic layers were washed with water and brine
  5. dry with materialdried over magnesium sulphate
  6. filtrationfiltered
  7. customevaporated in vacuo
  8. washeluting with 5 to 10% EtOAc in hexanes

出典と根拠

ORDレコード
ord-d37cb4d08d574798bbb03ca5e2fa5950
出典データセット
uspto-grants-2012_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08106091B2

反応ノート

読み込み中…

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