Acetic Acid → 5-Chloro-alpha-(2,4,6-trimethoxyphenyl)-2-(neopentylamino)benzyl alcohol

HRID 1791

반응식

HRID 1791 반응식
[NH2:1][C:2]1[CH:21]=[CH:20][C:19]([Cl:22])=[CH:18][C:3]=1[CH:4]([OH:17])[C:5]1[C:10]([O:11][CH3:12])=[CH:9][C:8]([O:13][CH3:14])=[CH:7][C:6]=1[O:15][CH3:16].[CH3:23][C:24]([CH3:28])([CH3:27])[CH:25]=O.C(O)(=O)C.C([BH3-])#N.[Na+]>C(O)C>[Cl:22][C:19]1[CH:20]=[CH:21][C:2]([NH:1][CH2:23][C:24]([CH3:28])([CH3:27])[CH3:25])=[C:3]([CH:18]=1)[CH:4]([OH:17])[C:5]1[C:6]([O:15][CH3:16])=[CH:7][C:8]([O:13][CH3:14])=[CH:9][C:10]=1[O:11][CH3:12]

참가 물질

6

반응물 4

HCID 176Acetic AcidHCID 12417PivalaldehydeHCID 5003444Sodium cyanoborohydrideHCID 544145002-Amino-5-chloro-alpha-(2,4,6-trimethoxyphenyl)benzyl alcohol

생성물 1

HCID 541447755-Chloro-alpha-(2,4,6-trimethoxyphenyl)-2-(neopentylamino)benzyl alcohol

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

After a solution of 2.5 g of 2-amino-5-chloro-α-(2,4,6-trimethoxyphenyl)benzyl alcohol, 1.01 ml of trimethylacetaldehyde and 0.56 g of acetic acid in 30 ml of ethanol was stirred at room temperature for 1.5 hours, 0.81 g of sodium cyanoborohydride was added, followed by stirring overnight. After concentration and subsequent dilution with water, the solution was extracted with ethyl acetate. After solvent removal, the residue was subjected to silica gel column chromatography to yield 2.2 g of a crystal.

후처리

  1. concentrationAfter concentration and subsequent dilution with water
  2. extractionthe solution was extracted with ethyl acetate
  3. customAfter solvent removal

출처 및 근거

ORD 기록
ord-775bed0ad28c49fbb6c1ce5df50c6d65
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05726306

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