Salicylaldehyde → HCID 53250564, 화합물

HRID 2169998

반응식

HRID 2169998 반응식
C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].[CH3:15][O:16][C:17]1[N:22]=[C:21]([NH2:23])[CH:20]=[CH:19][CH:18]=1.[OH:24][C:25]1[CH:32]=[CH:31][CH:30]=[CH:29][C:26]=1[CH:27]=O>O1CCCC1>[CH3:15][O:16][C:17]1[N:22]=[C:21]([NH:23][CH2:27][C:26]2[CH:29]=[CH:30][CH:31]=[CH:32][C:25]=2[OH:24])[CH:20]=[CH:19][CH:18]=1

참가 물질

5

반응물 3

HCID 6998Salicylaldehyde2회HCID 5800532-Amino-6-methoxypyridine2회HCID 5049666Sodium triacetoxyborohydride

생성물 1

HCID 53250564HCID 53250564, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

512 mg (2.41 mmol, 1.5 eq) of sodium triacetoxyborohydride are added to a solution of 200 mg (1.61 mmol, 1 eq) of 6-methoxypyridin-2-ylamine (starting material 1) and 236 mg (2.41 mmol, 1 eq) of 2-hydroxybenzaldehyde (starting material 2) in 20 ml of tetrahydrofuran. The solution is stirred at room temperature for 48 h. It is evaporated and the residue is taken up in 100 ml of dichloromethane and then extracted with a saturated aqueous solution of ammonium chloride. The aqueous phase is extracted twice with dichloromethane. The organic phases are combined and dried over sodium sulphate. The residue is chromatographed on silica gel (5/95 ethyl acetate/heptane). 2-[(6-methoxypyridin-2-ylamino)methyl]phenol is obtained in the form of a white solid. Melting point=103° C.

후처리

  1. customIt is evaporated
  2. extractionextracted with a saturated aqueous solution of ammonium chloride
  3. extractionThe aqueous phase is extracted twice with dichloromethane
  4. dry with materialdried over sodium sulphate
  5. customThe residue is chromatographed on silica gel (5/95 ethyl acetate/heptane)

출처 및 근거

ORD 기록
ord-eb5da2db59fa4c4ba1211fd2a8aac93e
출처 데이터셋
uspto-grants-2015_06
특허 번호
US09050266B2

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