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Trifluoroacetic acid → HCID 178448284、化合物

HRID 1011075
ノート
印刷プレビュー

反応式

HRID 1011075 の反応式
[CH3:1][C@@H:2]([O:6][C:7]1[N:15]=[C:14]2[C:10]([N:11]=[C:12]([O:22][CH3:23])[N:13]2C2CCCCO2)=[C:9]([NH2:24])[N:8]=1)[CH2:3][CH2:4][CH3:5].[F:25][C:26]([F:31])([F:30])[C:27]([OH:29])=[O:28]>CO.C(OCC)(=O)C>[F:25][C:26]([F:31])([F:30])[C:27]([OH:29])=[O:28].[CH3:1][C@@H:2]([O:6][C:7]1[NH:8][C:9]([NH2:24])=[C:10]2[C:14]([N:15]=1)=[N:13][C:12]([O:22][CH3:23])=[N:11]2)[CH2:3][CH2:4][CH3:5]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 6422Trifluoroacetic acidHCID 576995882-{[(1R)-1-Methylbutyl]oxy}-8-(methyloxy)-9-(tetrahydro-2H-pyran-2-yl)-9H-purin-6-amine

生成物 1

HCID 178448284HCID 178448284、化合物収率 73.6%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 8857Ethyl Acetate溶媒

実験手順

To a solution of 2-{[(1R)-1-methylbutyl]oxy}-8-(methyloxy)-9-(tetrahydro-2H-pyran-2-yl)-9H-purin-6-amine (4.8 g, 14.31 mmol) in methanol (100 ml) was added trifluoroacetic acid (8 ml, 104 mmol). The reaction mixture was stirred at room temperature for 72 hours. The solvent was removed in vacuo to give a pale yellow solid which was suspended in ethyl acetate (30 ml). The precipitate was filtered off and washed with further ethyl acetate until the filtrate was colourless. The remaining solid was dried by air and then in vacuo to give the title compound as a cream solid (3.85 g).

後処理

  1. customThe solvent was removed in vacuo
  2. customto give a pale yellow solid which
  3. filtrationThe precipitate was filtered off
  4. washwashed with further ethyl acetate until the filtrate
  5. customThe remaining solid was dried by air

出典と根拠

ORDレコード
ord-f7a0f0cf1ec649c59c004d1d0d35cf8b
出典データセット
uspto-grants-2011_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07977344B2

反応ノート

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