Water → 2-(Hydroxymethyl)-7-methoxy-9H-xanthen-9-OL

HRID 436000

反応式

HRID 436000 の反応式
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH3:7][O:8][C:9]1[CH:22]=[C:21]2[C:12]([O:13][C:14]3[CH:15]=[CH:16][C:17]([C:24](OCC)=[O:25])=[CH:18][C:19]=3[C:20]2=[O:23])=[CH:11][CH:10]=1.O.[O-]S([O-])(=O)=O.[Mg+2]>C1COCC1>[OH:23][CH:20]1[C:19]2[CH:18]=[C:17]([CH2:24][OH:25])[CH:16]=[CH:15][C:14]=2[O:13][C:12]2[C:21]1=[CH:22][C:9]([O:8][CH3:7])=[CH:10][CH:11]=2

参加物

6

反応物 4

HCID 962WaterHCID 24083Sulfuric acid magnesium salt (1:1)HCID 21226445Aluminium lithium hydrideHCID 21455094Ethyl 7-methoxy-9-oxoxanthene-2-carboxylate

生成物 1

HCID 214550952-(Hydroxymethyl)-7-methoxy-9H-xanthen-9-OL収率 84%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

Lithium aluminum hydride (500 mg) was added to a stirred solution of ethyl 7-methoxy-9-oxoxanthene-2-carboxylate (1g) in THF (100 ml). The reaction mixture was stirred at room temperature under nitrogen for 5 hours. Water and MgSO4 were added. The inorganic solids were filtered off and washed with ethyl acetate. The filtrate and washings were combined and evaporated to give the crude product. Recrystallization from ethyl acetate gave white crystals (0.82 g, 84%), mp. 142°-143°.

後処理

  1. filtrationThe inorganic solids were filtered off
  2. washwashed with ethyl acetate
  3. customevaporated
  4. customto give the crude product
  5. customRecrystallization from ethyl acetate

出典と根拠

ORDレコード
ord-67a38b1b31974630bd45356f0540d6db
出典データセット
uspto-grants-1977_02
特許番号
US04007205

関連ノート

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