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HCID 69271340、化合物 → HCID 69271247、化合物

HRID 2222382
ノート
印刷プレビュー

反応式

HRID 2222382 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5](/[C:11](=[CH:14]/[C:15]2[CH:20]=[CH:19][C:18]([C@@H:21]3[O:29][C@H:28]([CH2:30][OH:31])[C@@H:26]([OH:27])[C@H:24]([OH:25])[C@H:22]3[OH:23])=[CH:17][CH:16]=2)/[C:12]#[N:13])[CH:6]=[CH:7][C:8]=1[O:9][CH3:10].[P:32](Cl)(=[O:40])([O-:39])[O:33]CC(Cl)(Cl)Cl>N1C=CC=CC=1>[CH3:1][O:2][C:3]1[CH:4]=[C:5](/[C:11](=[CH:14]/[C:15]2[CH:16]=[CH:17][C:18]([C@@H:21]3[O:29][C@H:28]([CH2:30][O:31][P:32]([OH:40])([OH:39])=[O:33])[C@@H:26]([OH:27])[C@H:24]([OH:25])[C@H:22]3[OH:23])=[CH:19][CH:20]=2)/[C:12]#[N:13])[CH:6]=[CH:7][C:8]=1[O:9][CH3:10]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 69271340HCID 69271340、化合物HCID 85564173HCID 85564173、化合物

生成物 1

HCID 69271247HCID 69271247、化合物収率 70%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

Compound 44 (100 mg) and (2,2,2-trichloroethyl) phosphorochloridate (256 mg) were dissolved in pyridine (2 mL), and the resultant solution was stirred for two hours. After completion of reaction, the resultant reaction mixture was concentrated to dryness under reduced pressure, followed by purification by means of silica gel chromatography employing a chloroform/methanol system. The thus-purified product was dissolved in a pyridine-acetic acid (4:1) solvent mixture, and zinc powder (140 mg) was added to the resultant solution, followed by stirring for two hours. After completion of reaction, the resultant reaction mixture was concentrated to dryness under reduced pressure, followed by purification by means of silica gel chromatography employing a chloroform/methanol system, to thereby produce the target product (83 mg, yield: 70%).

後処理

  1. customAfter completion of reaction
  2. customthe resultant reaction mixture
  3. concentrationwas concentrated to dryness under reduced pressure
  4. customfollowed by purification by means of silica gel chromatography
  5. dissolutionThe thus-purified product was dissolved in a pyridine-acetic acid (4:1) solvent mixture, and zinc powder (140 mg)
  6. additionwas added to the resultant solution
  7. customAfter completion of reaction
  8. customthe resultant reaction mixture
  9. concentrationwas concentrated to dryness under reduced pressure
  10. customfollowed by purification by means of silica gel chromatography

出典と根拠

ORDレコード
ord-a01ce0428b0549558f3ce32d8460230a
出典データセット
uspto-grants-2008_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07371773B2

反応ノート

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