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Dicyclohexylcarbodiimide → (R)-((R)-quinuclidin-3-yl) 2-(tert-butoxycarbonylamino)-2-phenylacetate

HRID 2279935
ノート
印刷プレビュー

反応式

HRID 2279935 の反応式
[C:1]([O:5][C:6]([NH:8][C@H:9]([C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1)[C:10]([OH:12])=[O:11])=[O:7])([CH3:4])([CH3:3])[CH3:2].[N:19]12[CH2:26][CH2:25][CH:22]([CH2:23][CH2:24]1)[C@@H:21](O)[CH2:20]2.C1(N=C=NC2CCCCC2)CCCCC1.O.ON1C2C=CC=CC=2N=N1>O1CCCC1>[C:1]([O:5][C:6]([NH:8][C@H:9]([C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1)[C:10]([O:12][C@@H:21]1[CH:22]2[CH2:25][CH2:26][N:19]([CH2:24][CH2:23]2)[CH2:20]1)=[O:11])=[O:7])([CH3:4])([CH3:2])[CH3:3]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 10868DicyclohexylcarbodiimideHCID 914043-Quinuclidinol, (-)-HCID 2755953(2R)-2-{[(tert-butoxy)carbonyl]amino}-2-phenylacetic acidHCID 27960291-Hydroxybenzotriazole hydrate

生成物 1

HCID 67607970(R)-((R)-quinuclidin-3-yl) 2-(tert-butoxycarbonylamino)-2-phenylacetate収率 17%

試薬・触媒・溶媒 1

HCID 8028
Tetrahydrofuran
溶媒

実験手順

A mixture of (R)-2-((tert-Butoxycarbonyl)amino)-2-phenylacetic acid (5.0 g, 19.9 mmol), (R) enantiomeric pure form commercially available or obtainable from I-41 with known methods e.g. chiral preparative SFC, (R)-quinuclidin-3-ol (3.8 g, 29.8 mmol), N,N′-Dicyclohexylcarbodiimide (4.72 g, 22.9 mmol) and 1-hydroxybenzotriazole hydrate (3.09 g, 22.9 mmol) in tetrahydrofuran (175 mL) was stirred at room temperature for 18 h. After this time the reaction mixture was filtered through a pad of Celite® and concentrated in vacuo. The residue was partitioned between ethyl acetate (100 mL) and 10% aqueous sodium carbonate solution (50 mL), and the organic fractions were dried over magnesium sulfate, filtered and the solvent was removed in vacuo. Trituration with cold methanol gave the title compound as a white solid (898 mg, 17%) as a single diastereoisomer.

後処理

  1. filtrationAfter this time the reaction mixture was filtered through a pad of Celite®
  2. concentrationconcentrated in vacuo
  3. customThe residue was partitioned between ethyl acetate (100 mL) and 10% aqueous sodium carbonate solution (50 mL)
  4. dry with materialthe organic fractions were dried over magnesium sulfate
  5. filtrationfiltered
  6. customthe solvent was removed in vacuo

出典と根拠

ORDレコード
ord-aacf24cd20dd4b3aac892368da0ffcc1
出典データセット
uspto-grants-2015_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09133185B2

反応ノート

読み込み中…

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