Potassium Carbonate → 3-(5'-Hydroxymethyl-2'-furyl)-1-benzylindazole

HRID 1594250노트

반응식

HRID 1594250 반응식
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH2:7]([N:14]1[C:22]2[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=2)[C:16]([C:23]2[O:24][C:25]([C:28](OCC)=[O:29])=[CH:26][CH:27]=2)=[N:15]1)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.C(=O)([O-])[O-].[K+].[K+]>C1COCC1>[CH2:7]([N:14]1[C:22]2[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=2)[C:16]([C:23]2[O:24][C:25]([CH2:28][OH:29])=[CH:26][CH:27]=2)=[N:15]1)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 15408136HCID 15408136, 화합물HCID 21226445Aluminium lithium hydride

생성물 1

HCID 57123-(5'-Hydroxymethyl-2'-furyl)-1-benzylindazole

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

2.06 g (54.6 mmol) of lithium aluminum hydride were initially charged in 250 ml of absolute THF, and a solution of 18.8 g (54.6 mmol) of 1-benzyl-3-(5-ethoxycarbonyl-2-furyl)indazole in 250 ml of THF was added dropwise. After 45 min the mixture was admixed with 25% strength potassium carbonate solution and stirred at RT for 30 min and the precipitate was filtered off with suction and washed with THF. The combined organic phases were concentrated using a rotary evaporator and the residue was recrystallized from isopropanol. This gave 11.0 g (67%) of the title compound. m.p.: 113-114° C.

후처리

  1. filtrationthe precipitate was filtered off with suction
  2. washwashed with THF
  3. concentrationThe combined organic phases were concentrated
  4. customa rotary evaporator
  5. customthe residue was recrystallized from isopropanol

출처 및 근거

ORD 기록
ord-61e5a6f3f44e412c948097b21d25aaa9
출처 데이터셋
uspto-grants-2007_11
특허 번호
US07300950B2

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