1,2-Dichloroethane → Methyl 14-cyclohexyl-5-methyl-5,6,7,8-tetrahydroindolo[1,2-e][1,5]benzodiazocine-11-carboxylate

HRID 1444633ノート

反応式

HRID 1444633 の反応式
[CH:1]1([C:7]2[C:8]3[CH:9]=[CH:10][C:11]([C:26]([O:28][CH3:29])=[O:27])=[CH:12][C:13]=3[N:14]3[C:21]=2[C:20]2[CH:22]=[CH:23][CH:24]=[CH:25][C:19]=2[NH:18][CH2:17][CH2:16][CH2:15]3)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.Cl[CH2:31]CCl.C=O.[BH-](OC(C)=O)(OC(C)=O)OC(C)=O.[Na+]>CCOC(C)=O>[CH:1]1([C:7]2[C:8]3[CH:9]=[CH:10][C:11]([C:26]([O:28][CH3:29])=[O:27])=[CH:12][C:13]=3[N:14]3[C:21]=2[C:20]2[CH:22]=[CH:23][CH:24]=[CH:25][C:19]=2[N:18]([CH3:31])[CH2:17][CH2:16][CH2:15]3)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6]1

参加物

6

反応物 4

HCID 111,2-DichloroethaneHCID 712FormaldehydeHCID 5049666Sodium triacetoxyborohydrideHCID 68699880HCID 68699880、化合物

生成物 1

HCID 68695685Methyl 14-cyclohexyl-5-methyl-5,6,7,8-tetrahydroindolo[1,2-e][1,5]benzodiazocine-11-carboxylate

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

To a solution of methyl 14-cyclohexyl-5,6,7,8-tetrahydroindolo[1,2-e][1,5]benzodiazocine-11-carboxylate in DCE (0.05 M) 1 eq of formaldehyde (37 wt. % sol. in H2O) and 2 eq of NaBH(OAc)3 were added and the solution stirred at RT for 1 h. The reaction mixture was diluted with EtOAc. The organic phase was washed with NaHCO3 (s.s.) and brine. The organic phase was dried over Na2SO4 filtered and concentrated in vacuo. The title compound was used directly in the next step; MS (ES+) m/z 403 (M+H)+.

後処理

  1. washThe organic phase was washed with NaHCO3 (s.s.) and brine
  2. dry with materialThe organic phase was dried over Na2SO4
  3. filtrationfiltered
  4. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-e916ada497b948d08e8071c2874dc42a
出典データセット
uspto-grants-2010_02
特許番号
US07662809B2

反応ノート

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