Ethanol → [2-(6-Methoxy-quinazolin-4-yl)-ethyl]-1,4-dioxa-spiro[4.5]decan-8-ol

HRID 1354206ノート

反応式

HRID 1354206 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][CH:12]=1)[N:9]=[CH:8][N:7]=[C:6]2[C:13]#[C:14][C:15]1([OH:25])[CH2:24]CC2(OCCO2)CC1.[CH3:26][CH2:27][OH:28]>C1COCC1.[Pt]=O>[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][CH:12]=1)[N:9]=[CH:8][N:7]=[C:6]2[CH2:13][CH2:14][CH:15]1[CH2:24][O:28][C:27]2([CH2:11][CH2:12][CH:3]([OH:2])[CH2:4][CH2:26]2)[O:25]1

参加物

5

反応物 2

HCID 702EthanolHCID 211046688-(6-Methoxy-quinazolin-4-ylethynyl)-1,4-dioxa-spiro[4.5]decan-8-ol

生成物 1

HCID 86603231[2-(6-Methoxy-quinazolin-4-yl)-ethyl]-1,4-dioxa-spiro[4.5]decan-8-ol

試薬・触媒・溶媒 2

HCID 82844Platinum oxide (PtO)触媒HCID 8028Tetrahydrofuran溶媒

実験手順

Platinum oxide (0.46 g) was added to a solution of 8-(6-methoxy-quinazolin-4-ylethynyl)-1,4-dioxa-spiro[4.5]decan-8-ol (0.96 g, 2.88 mmol) in EtOH (40 ml) and THF (10 ml), and hydrogenation was carried out under a hydrogen atmosphere (1 bar). The reaction mixture was stirred in the presence of activated carbon (5 g) and filtered. The filtrate was concentrated to dryness by rotary evaporation. The residue was purified by column chromatography on silica gel (EtOAc and then EtOAc:MeOH 9/1).

後処理

  1. filtrationfiltered
  2. concentrationThe filtrate was concentrated to dryness by rotary evaporation
  3. customThe residue was purified by column chromatography on silica gel (EtOAc

出典と根拠

ORDレコード
ord-5d443ac33af84a09a6b4388cf7724908
出典データセット
uspto-grants-2007_05
特許番号
US07223776B2

反応ノート

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