Sodium Acetate → HCID 18172391、化合物

HRID 397088

反応式

HRID 397088 の反応式
[N:1]1([CH2:6][CH2:7][O:8][C:9]2[CH:14]=[CH:13][C:12]([CH:15]3[C:24]4[C:19](=[CH:20][C:21]([OH:25])=[CH:22][CH:23]=4)[CH2:18][CH2:17][NH:16]3)=[CH:11][CH:10]=2)[CH2:5][CH2:4][CH2:3][CH2:2]1.[N:26]1([C:31]2[CH:38]=[CH:37][C:34]([CH:35]=O)=[CH:33][CH:32]=2)[CH:30]=[CH:29][N:28]=[CH:27]1.CC([O-])=O.[Na+].C([BH3-])#N.[Na+]>CO>[N:26]1([C:31]2[CH:38]=[CH:37][C:34]([CH2:35][N:16]3[CH2:17][CH2:18][C:19]4[C:24](=[CH:23][CH:22]=[C:21]([OH:25])[CH:20]=4)[CH:15]3[C:12]3[CH:13]=[CH:14][C:9]([O:8][CH2:7][CH2:6][N:1]4[CH2:5][CH2:4][CH2:3][CH2:2]4)=[CH:10][CH:11]=3)=[CH:33][CH:32]=2)[CH:30]=[CH:29][N:28]=[CH:27]1

参加物

6

反応物 4

HCID 517045Sodium AcetateHCID 7365304-(1H-imidazol-1-yl)benzaldehydeHCID 5003444Sodium cyanoborohydrideHCID 181724491-[4-(2-Pyrrolidin-1-yl-ethoxy)phenyl]-1,2,3,4-tetrahydroisoquinolin-6-ol

生成物 1

HCID 18172391HCID 18172391、化合物収率 112.3%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A solution of 1-[4-(2-pyrrolidin-1-yl-ethoxy)phenyl]-1,2,3,4-tetrahydroisoquinolin-6-ol (0.023 g, 0.067 mmol), 4-imidazol-1-yl-benzaldehyde (0.011 g, 0.063 mmol), NaOAc (0.011 g, 0.14 mmol), and sodium cyanoborohydride (0.004 g, 0.063 mmol) in MeOH (2.0 ml) was stirred at rt for 18 hr. The reaction mixture was evaporated in vacuo to a yellow residue that was dissolved in EtOAc (5 ml) and washed first with sat. NaHCO3 solution (5 ml) and then with H2O (5 ml). The organic solution was dried over MgSO4 and evaporated to give 0.035 g of yellow residue. Purification by preparative TLC, eluting with EtOAc:MeOH (7:3), gave 0.007 g (23% yield) of white solid.

後処理

  1. customThe reaction mixture was evaporated in vacuo to a yellow residue that
  2. dissolutionwas dissolved in EtOAc (5 ml)
  3. washwashed first with sat. NaHCO3 solution (5 ml)
  4. dry with materialThe organic solution was dried over MgSO4
  5. customevaporated

出典と根拠

ORDレコード
ord-ca3227ff177140879ce3c5041d487307
出典データセット
uspto-grants-2003_08
特許番号
US06608203B2

関連ノート

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