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Triethylamine → ethyl 8-(2-Ethyl-6-methylbenzylamino)-3-methylimidazo[1,2-a]pyridin-2-carboxylate

HRID 1166169
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HRID 1166169 반응식
[NH2:1][C:2]1[C:3]2[N:4]([C:8]([CH3:16])=[C:9]([C:11]([O:13][CH2:14][CH3:15])=[O:12])[N:10]=2)[CH:5]=[CH:6][CH:7]=1.[CH2:17]([C:19]1[CH:26]=[CH:25][CH:24]=[C:23]([CH3:27])[C:20]=1[CH:21]=O)[CH3:18].C([BH3-])#N.[Na+].C(N(CC)CC)C>CO.[Cl-].[Zn+2].[Cl-]>[CH2:17]([C:19]1[CH:26]=[CH:25][CH:24]=[C:23]([CH3:27])[C:20]=1[CH2:21][NH:1][C:2]1[C:3]2[N:4]([C:8]([CH3:16])=[C:9]([C:11]([O:13][CH2:14][CH3:15])=[O:12])[N:10]=2)[CH:5]=[CH:6][CH:7]=1)[CH3:18]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 8471TriethylamineHCID 5003444Sodium cyanoborohydrideHCID 22672637Ethyl 8-amino-3-methylimidazo[1,2-a]pyridine-2-carboxylateHCID 229974692-Ethyl-6-methylbenzaldehyde

생성물 1

HCID 22997468ethyl 8-(2-Ethyl-6-methylbenzylamino)-3-methylimidazo[1,2-a]pyridin-2-carboxylate수율 8.1%

시약·촉매·용매 2

HCID 3007855
Zincchloride
촉매
HCID 887Methanol용매2회

실험 절차

To a stirred mixture of ethyl 8-amino-3-methylimidazo[1,2-a]pyridin-2-carboxylate (1.53 g, 7.0 mmol) in methanol (25 ml) were added 2-ethyl-6-methylbenzaldehyde (1.1 g, 7.1 mmol), zinc(II)chloride (1.1 g, 8.0 mmol) in methanol (10 ml) and sodium cyanoborohydride (0.5 g, 8.0 mmol). The reaction mixture was refluxed for 4 h. and then stirred at room temperature for 20 h. Triethylamine (2.5 ml) was added and the mixture was stirred for 30 min. and evaporated under reduced pressure. Purification of the residue by column chromatography twice on silica gel using 1) methylene chloride:methanol (95:5) 2) heptane:isopropyl ether (1:5) as eluent gave 0.2 g (8%) of the title compound.

후처리

  1. temperatureThe reaction mixture was refluxed for 4 h.
  2. stirringthe mixture was stirred for 30 min.
  3. customevaporated under reduced pressure
  4. customPurification of the residue by column chromatography twice on silica gel using 1) methylene chloride:methanol (95:5) 2) heptane:isopropyl ether (1:5) as eluent

출처 및 근거

ORD 기록
ord-80da9f086b924dc391ffbf26a527ba0c
출처 데이터셋
uspto-grants-2003_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06613775B1

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