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Water → HCID 21717366、化合物

HRID 1386065
ノート
印刷プレビュー

反応式

HRID 1386065 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 2724148Sodium potassium tartrate tetrahydrateHCID 16684438Red-AlHCID 21717328HCID 21717328、化合物

生成物 1

HCID 21717366HCID 21717366、化合物収率 62%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒3 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-4dfa35d364ed48749511375dc026f43c
出典データセット
uspto-grants-2001_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06265415B1

反応ノート

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