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Water → HCID 21717366, 화합물

HRID 1386065
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HRID 1386065 반응식
[C:1]([C:6]1[N:10]2[CH:11]=[C:12]([CH3:25])[CH:13]=[C:14]([NH:15][CH2:16][C:17]3[C:22]([CH3:23])=[CH:21][CH:20]=[CH:19][C:18]=3[CH3:24])[C:9]2=[N:8][C:7]=1[CH3:26])(OCC)=[O:2].COCCO[AlH2-]OCCOC.[Na+].O.O.O.O.C(C(C(C([O-])=O)O)O)([O-])=O.[K+].[Na+].O>C1(C)C=CC=CC=1>[CH3:26][C:7]1[N:8]=[C:9]2[C:14]([NH:15][CH2:16][C:17]3[C:22]([CH3:23])=[CH:21][CH:20]=[CH:19][C:18]=3[CH3:24])=[CH:13][C:12]([CH3:25])=[CH:11][N:10]2[C:6]=1[CH2:1][OH:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 2724148Sodium potassium tartrate tetrahydrateHCID 16684438Red-AlHCID 21717328HCID 21717328, 화합물

생성물 1

HCID 21717366HCID 21717366, 화합물수율 62%

시약·촉매·용매 1

HCID 1140Toluene용매3회

실험 절차

A solution of 3-carboethoxy-2,6-dimethyl-8-(2,6-dimethylbenzylamino)imidazo[1,2-a]pyridine (0.4 g, 1.1 mmol) in 10 ml toluene was cold with ice- water, Red-AL 65% in to toluene (2.1 g, 6.6 mmol) was added after 30 min. The solution was stirred for 2 h at room temperature. 10 ml of Rochelle-salt solution (sodium potassium tartrate tetrahydrate, 35 g/250 ml water) was added dropwise, 10 ml toluene was added, the organic layer was separated and washed with water, dried over sodium sulfate and evaporated under reduced pressure. The residue was purified by column chromatography on silica gel, eluent dichloromethane:methanol 9:1, to give 0.21 g, (62%) of the title compound.

후처리

  1. additionwas added after 30 min
  2. customthe organic layer was separated
  3. washwashed with water
  4. dry with materialdried over sodium sulfate
  5. customevaporated under reduced pressure
  6. customThe residue was purified by column chromatography on silica gel, eluent dichloromethane:methanol 9:1

출처 및 근거

ORD 기록
ord-4dfa35d364ed48749511375dc026f43c
출처 데이터셋
uspto-grants-2001_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06265415B1

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