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Borohydride → HCID 13304947, 화합물

HRID 371394
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HRID 371394 반응식
[BH4-].[Li+].[CH2:3]([C:5]1[C:6]([O:20][CH3:21])=[N:7][C:8]2[N:9]([CH:12]=[C:13]([C:15](OCC)=[O:16])[N:14]=2)[C:10]=1[CH3:11])[CH3:4].[BH4-]>O1CCCC1>[CH2:3]([C:5]1[C:6]([O:20][CH3:21])=[N:7][C:8]2[N:9]([CH:12]=[C:13]([CH2:15][OH:16])[N:14]=2)[C:10]=1[CH3:11])[CH3:4]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 28123BorohydrideHCID 4148881Lithium borohydrideHCID 13304946HCID 13304946, 화합물

생성물 1

HCID 13304947HCID 13304947, 화합물수율 93%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

11.55 g (0.525 mol) of lithium borohydride were added portionwise over 1 hour to a stirred solution of 19.7 g (75 mmol) of ethyl 6-ethyl-7-methoxy-5-methylimidazo[1,2-a]pyrimidine-2-carboxylate in 300 ml of dry tetrahydrofuran and after stirring at room temperature for 18 hours the excess borohydride was destroyed by dropwise addition of 300 ml of saturated sodium chloride solution. Then, the mixture was stirred for 30 minutes before separating the organic layer. The aqueous layer was extracted with chloroform and the combined extracts were dried over anhydrous magnesium sulfate and evaporated to dryness under reduced pressure to obtain 15.4 g (6-ethyl-7-methoxy-5-methylimidazo[1,2-a]pyrimidin-2-yl)methanol (93% yield as a white crystalline solid melting at 186-188° C. (decomp.).

후처리

  1. customwas destroyed by dropwise addition of 300 ml of saturated sodium chloride solution
  2. custombefore separating the organic layer
  3. extractionThe aqueous layer was extracted with chloroform
  4. dry with materialthe combined extracts were dried over anhydrous magnesium sulfate
  5. customevaporated to dryness under reduced pressure

출처 및 근거

ORD 기록
ord-cc3e8e602ebb4b37b96629719084e6df
출처 데이터셋
uspto-grants-1985_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04532243

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