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Bicarbonate Ion → HCID 11493075, 화합물

HRID 1781570
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HRID 1781570 반응식
I[C:2]1[C:3](=[O:17])[NH:4][C:5](=[O:16])[N:6]([CH:15]=1)[C@@H:7]1[O:14][C@H:11]([CH2:12][OH:13])[C@@H:9]([OH:10])[CH2:8]1.[CH:18]#[C:19][CH2:20][CH2:21][CH3:22].CO.C(=O)(O)[O-]>[Pd].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[Cu]I.C(Cl)Cl>[C:18]([C:2]1[C:3](=[O:17])[NH:4][C:5](=[O:16])[N:6]([CH:15]=1)[C@@H:7]1[O:14][C@H:11]([CH2:12][OH:13])[C@@H:9]([OH:10])[CH2:8]1)#[C:19][CH2:20][CH2:21][CH3:22]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 769Bicarbonate IonHCID 887MethanolHCID 5905IdoxuridineHCID 123091-Pentyne

생성물 1

HCID 11493075HCID 11493075, 화합물수율 81.9%

시약·촉매·용매 3

HCID 24350Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)
촉매
HCID 11979704Tetrakis(triphenylphosphine)palladium촉매
HCID 6344Dichloromethane용매

실험 절차

This compound was prepared by the same procedure that Hobbs, F. W. J., J Org Chem (1989) 54: 3420-3422, used for the preparation of other alkynyl substituted nucleosides. A mixture of 30.0 g (84.7 mmol) of 5-iodo-2'deoxyuridine (purchased from Sigma), 23.6 mL of 1-pentyne (Aldrich), 9.79 g of tetrakis (triphenylphosphine) palladium (0) (Aldrich), and 3.23 g of copper (I) iodide were stirred at room temperature for 26 h. To the reaction was added 250 mL of MeOH and 250 mL of CH2Cl2. The mixture was neutralized with Dowex 1 x 8-200 (bicarbonate form) ion exchange resin. The mixture was filtered and concentrated. The residue was partitioned between H2O and CH2Cl2. The aqueous layer was extracted three times with CH2Cl2 and then concentrated. Purification of the crude product by column chromatography afforded 20.4 g (81.9% yield) of product.

후처리

  1. customThis compound was prepared by the same procedure that Hobbs, F
  2. filtrationThe mixture was filtered
  3. concentrationconcentrated
  4. customThe residue was partitioned between H2O and CH2Cl2
  5. extractionThe aqueous layer was extracted three times with CH2Cl2
  6. concentrationconcentrated
  7. customPurification of the crude product by column chromatography

출처 및 근거

ORD 기록
ord-f301d0b9494940d59d0901c5a8aebf22
출처 데이터셋
uspto-grants-1997_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05633360

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