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

HRID 436000

반응식

HRID 436000 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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°.

후처리

  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

출처 및 근거

ORD 기록
ord-67a38b1b31974630bd45356f0540d6db
출처 데이터셋
uspto-grants-1977_02
특허 번호
US04007205

연결된 노트

불러오는 중…