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Benzene → (1R,3R)-methyl 1-amino-3-(4-(3-(benzyloxy)prop-1-ynyl)phenyl)cyclopentanecarboxylate

HRID 1511845
ノート
印刷プレビュー

反応式

HRID 1511845 の反応式
[NH2:1][C@:2]1([C:14]([O:16][CH3:17])=[O:15])[CH2:6][CH2:5][C@@H:4]([C:7]2[CH:12]=[CH:11][C:10](Br)=[CH:9][CH:8]=2)[CH2:3]1.C(O)(=O)[C@@H]([C@H](C(O)=O)O)O.N1CCCCC1.[CH2:34]([O:37][CH2:38][C:39]1[CH:44]=[CH:43][CH:42]=[CH:41][CH:40]=1)[C:35]#[CH:36].C1C=CC=CC=1>[Cu]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.C1COCC1>[NH2:1][C@:2]1([C:14]([O:16][CH3:17])=[O:15])[CH2:6][CH2:5][C@@H:4]([C:7]2[CH:12]=[CH:11][C:10]([C:36]#[C:35][CH2:34][O:37][CH2:38][C:39]3[CH:44]=[CH:43][CH:42]=[CH:41][CH:40]=3)=[CH:9][CH:8]=2)[CH2:3]1
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 5

HCID 241BenzeneHCID 8082PiperidineHCID 444305L-Tartaric acidHCID 6917484((Prop-2-yn-1-yloxy)methyl)benzeneHCID 25002100(1R,3R)-methyl 1-amino-3-(4-bromophenyl)cyclopentanecarboxylate

生成物 1

HCID 57554604(1R,3R)-methyl 1-amino-3-(4-(3-(benzyloxy)prop-1-ynyl)phenyl)cyclopentanecarboxylate
収率 86%

試薬・触媒・溶媒 3

HCID 24350Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)触媒HCID 178418476HCID 178418476、化合物触媒HCID 8028Tetrahydrofuran溶媒

実験手順

A round bottomed flask was charged with (1R,3R)-methyl 1-amino-3-(4-bromophenyl)cyclopentanecarboxylate, 0.5 L-tartaric acid 2 (30 g, 80 mmol), copper(I) iodide (0.153 g, 0.804 mmol), bis(triphenylphosphine)palladium(II) dichloride (2.82 g, 4.02 mmol) and THF (200 mL). The reaction mixture was purged with nitrogen. After about 15 minutes piperidine (35.8 mL, 362 mmol) and ((prop-2-ynyloxy)methyl)benzene (11.75 g, 80 mmol) were added and the reaction mixture was heated to about 65°. After about 2 hours additional (prop-2-ynyloxy)methyl)benzene (11.75 g, 80 mmol) was added. After about 8 hours the crude reaction mixture was partitioned between EtOAc and saturated NaHCO3. The organic layer was washed with brine, dried (Na2SO4) filtered, concentrated in vacuo and purified by flash chromatography on silica gel (eluting with EtOAC/Heptane followed by EtOAc/MeOH) to provide (1R,3R)-methyl 1-amino-3-(4-(3-(benzyloxy)prop-1-ynyl)phenyl)cyclopentanecarboxylate (25 g, 68.8 mmol, 86% yield) as a brown oil.

後処理

  1. customThe reaction mixture was purged with nitrogen
  2. temperaturethe reaction mixture was heated to about 65°
  3. customAfter about 8 hours the crude reaction mixture
  4. customwas partitioned between EtOAc and saturated NaHCO3
  5. washThe organic layer was washed with brine
  6. dry with materialdried (Na2SO4)
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo
  9. custompurified by flash chromatography on silica gel (eluting with EtOAC/Heptane followed by EtOAc/MeOH)

出典と根拠

ORDレコード
ord-e84b1045d13a416da5c88ccc3405c1f2
出典データセット
uspto-grants-2012_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08217027B2

反応ノート

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