Triethylamine → 4'-C-triethylsilylethynyl-3',5'-di-O-benzyluridine

HRID 2186318ノート

反応式

HRID 2186318 の反応式
[CH2:1]([Si:3]([C:8]#[C:9][C@:10]1([CH2:35][O:36][CH2:37][C:38]2[CH:43]=[CH:42][CH:41]=[CH:40][CH:39]=2)[O:14][C@@H:13]([N:15]2[CH:22]=[CH:21][C:19](=[O:20])[NH:18][C:16]2=[O:17])[C@H:12]([O:23]C(=O)C)[C@@H:11]1[O:27][CH2:28][C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1)([CH2:6][CH3:7])[CH2:4][CH3:5])[CH3:2].C(N(CC)CC)C>CO>[CH2:1]([Si:3]([C:8]#[C:9][C@:10]1([CH2:35][O:36][CH2:37][C:38]2[CH:39]=[CH:40][CH:41]=[CH:42][CH:43]=2)[O:14][C@@H:13]([N:15]2[CH:22]=[CH:21][C:19](=[O:20])[NH:18][C:16]2=[O:17])[C@H:12]([OH:23])[C@@H:11]1[O:27][CH2:28][C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1)([CH2:6][CH3:7])[CH2:4][CH3:5])[CH3:2]

参加物

4

反応物 2

HCID 8471TriethylamineHCID 10651295HCID 10651295、化合物

生成物 1

HCID 107455044'-C-triethylsilylethynyl-3',5'-di-O-benzyluridine

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Compound 7 (2.00 g, 3.3 mmol) was dissolved in methanol (90.0 ml), and triethylamine (10.0 ml) was added to the solution, followed by stirring for 48 hours at room temperature. The reaction mixture was concentrated through distillation under reduced pressure, and the residue was purified by means of silica gel column chromatography (silica gel 200 ml, eluent; n-hexane:ethyl acetate=1:1), to thereby yield a white powdery compound (Compound 8; 1.72 g, 3.06 mmol, 92.4%).

後処理

  1. concentrationThe reaction mixture was concentrated through distillation under reduced pressure
  2. customthe residue was purified by means of silica gel column chromatography (silica gel 200 ml, eluent; n-hexane:ethyl acetate=1:1)

出典と根拠

ORDレコード
ord-6b58d2a85cfe49cb9efcb16e19976245
出典データセット
uspto-grants-2002_06
特許番号
US06403568B1

反応ノート

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