反応式
[N:1]1([C:9]2[CH:14]=[CH:13][C:12]([C:15]3[CH:20]=[CH:19][C:18]([N:21]4[C:26](=[O:27])[CH:25]=[CH:24][CH:23]=[N:22]4)=[CH:17][CH:16]=3)=[CH:11][CH:10]=2)[CH2:5][CH2:4][C@@H:3]2[CH2:6][NH:7][CH2:8][C@H:2]12.C=O.[C:30](O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].Cl.[OH-].[Na+]>CC(N(C)C)=O>[CH3:30][N:7]1[CH2:6][C@@H:3]2[C@@H:2]([N:1]([C:9]3[CH:14]=[CH:13][C:12]([C:15]4[CH:20]=[CH:19][C:18]([N:21]5[C:26](=[O:27])[CH:25]=[CH:24][CH:23]=[N:22]5)=[CH:17][CH:16]=4)=[CH:11][CH:10]=3)[CH2:5][CH2:4]2)[CH2:8]1参加物
実験手順
To a stirred solution of the product of Example 1F (13.80 g, 31.41 mmol) in dimethylacetamide (500 mL) was added a solution of 37% aqueous formaldehyde (7.2 mL, 94.23 mmol, 3.0 equivalents) followed by sodium triacetoxyborohydride (20.0 g, 94.23 mmol, 3.0 equivalents). The mixture was stirred at 25+/−5° C. for 30 minutes during which the starting material was consumed, giving a clear solution. The mixture was diluted with 1N HCl (94 mL, 94 mmol, 3 equivalents) and stirred for one hour. The mixture was adjusted to pH 9.0+/−0.5 with 1N NaOH (335 mL). The mixture was stirred for 1 hour then filtered. The wet cake was washed with water and dried in a vacuum oven at about 50° C. to provide the title compound, 2-[4′-(3aR,6aR)-(5-methylhexahydropyrrolo[3,4-b]pyrrol-1(2H)-yl)-1,1′-biphenyl-4-yl ]pyridazin-3(2H)-one (10.40 g, 88.9%).
後処理
- customwas consumed
- customgiving a clear solution
- stirringstirred for one hour
- stirringThe mixture was stirred for 1 hour
- filtrationthen filtered
- washThe wet cake was washed with water
- customdried in a vacuum oven at about 50° C.
出典と根拠
- ORDレコード
- ord-a64e56aa2599406f8cb08490f2a1548c
- 出典データセット
- uspto-grants-2011_09
- 特許番号
- US08026240B2
関連ノート
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