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Water → HCID 22007318、化合物

HRID 323876
ノート
印刷プレビュー

反応式

HRID 323876 の反応式
C(=O)([O-])[O-].[K+].[K+].[CH3:7][N:8]1[C:16]2[N:15]=[CH:14][N:13]([C:17]([C:30]3[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=3)([C:24]3[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=3)[C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=3)[C:12]=2[C:11](=[O:36])[NH:10][C:9]1=[O:37].[CH2:38]([O:45][CH2:46]Cl)[C:39]1[CH:44]=[CH:43][CH:42]=[CH:41][CH:40]=1.O>CN(C)C=O>[CH2:38]([O:45][CH2:46][N:10]1[C:11](=[O:36])[C:12]2[N:13]([C:17]([C:24]3[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=3)([C:30]3[CH:31]=[CH:32][CH:33]=[CH:34][CH:35]=3)[C:18]3[CH:19]=[CH:20][CH:21]=[CH:22][CH:23]=3)[CH:14]=[N:15][C:16]=2[N:8]([CH3:7])[C:9]1=[O:37])[C:39]1[CH:44]=[CH:43][CH:42]=[CH:41][CH:40]=1
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 962WaterHCID 11430Potassium CarbonateHCID 137983Benzyl chloromethyl etherHCID 22007310HCID 22007310、化合物

生成物 1

HCID 22007318HCID 22007318、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

1.3 g (9.44 mmol) of potassium carbonate were added at 60° C. to a solution of 2.4 g (5.9 mmol) of 3-methyl-7-tritylxanthine from stage a) in 50 ml of dimethylformamide and the mixture was stirred at this temperature for one hour. 1.06 ml (7.67 mmol) of benzyloxymethyl chloride were then added dropwise and the mixture was stirred at 80° C. for 7 hours. 50 ml of water were then added and the mixture was extracted three times using 60 ml of methyl tert-butyl ether each time. The combined organic phases were washed twice with 30 ml of water each time, dried using magnesium sulfate and concentrated under reduced pressure. The crude product was purified by flash chromatography on a silica gel column, heptane/ethyl acetate (3/2).

後処理

  1. stirringthe mixture was stirred at 80° C. for 7 hours
  2. extractionthe mixture was extracted three times
  3. washThe combined organic phases were washed twice with 30 ml of water each time
  4. customdried
  5. concentrationconcentrated under reduced pressure
  6. customThe crude product was purified by flash chromatography on a silica gel column, heptane/ethyl acetate (3/2)

出典と根拠

ORDレコード
ord-43c493a903f4471eb3efe46a36545df3
出典データセット
uspto-grants-2001_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06214992B1

反応ノート

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