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Acetic Acid → 6-[(4R)-4-({[3-(6,7-Difluoro-2-oxoquinoxalin-1(2H)-yl)propyl]amino}methyl)-2-oxopyrrolidin-1-yl]-2H-pyrido[3,2-b][1,4]oxazin-3(4H)-one

HRID 1847085
ノート
印刷プレビュー

反応式

HRID 1847085 の反応式
C(O)(=O)C.[F:5][C:6]1[CH:7]=[C:8]2[C:13](=[CH:14][C:15]=1[F:16])[N:12]([CH2:17][CH2:18][CH:19]=O)[C:11](=[O:21])[CH:10]=[N:9]2.[NH2:22][CH2:23][C@@H:24]1[CH2:28][N:27]([C:29]2[CH:30]=[CH:31][C:32]3[O:33][CH2:34][C:35](=[O:39])[NH:36][C:37]=3[N:38]=2)[C:26](=[O:40])[CH2:25]1.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].C(=O)([O-])O.[Na+]>CO>[F:5][C:6]1[CH:7]=[C:8]2[C:13](=[CH:14][C:15]=1[F:16])[N:12]([CH2:17][CH2:18][CH2:19][NH:22][CH2:23][C@@H:24]1[CH2:28][N:27]([C:29]3[CH:30]=[CH:31][C:32]4[O:33][CH2:34][C:35](=[O:39])[NH:36][C:37]=4[N:38]=3)[C:26](=[O:40])[CH2:25]1)[C:11](=[O:21])[CH:10]=[N:9]2
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 5

HCID 176Acetic AcidHCID 516892Sodium BicarbonateHCID 5049666Sodium triacetoxyborohydrideHCID 867249736-[(4R)-4-(Aminomethyl)-2-oxopyrrolidin-1-yl]-2H-pyrido[3,2-b][1,4]oxazin-3(4H)-oneHCID 867250073-(6,7-Difluoro-2-oxoquinoxalin-1(2H)-yl)propanal

生成物 1

HCID 86725008
6-[(4R)-4-({[3-(6,7-Difluoro-2-oxoquinoxalin-1(2H)-yl)propyl]amino}methyl)-2-oxopyrrolidin-1-yl]-2H-pyrido[3,2-b][1,4]oxazin-3(4H)-one
収率 7%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Acetic acid (32 mg, 0.58 mmol) was added to a mixture of 3-(6,7-difluoro-2-oxoquinoxalin-1(2H)-yl)propanal (0.1 g, 0.45 mmol), 6-[(4R)-4-(aminomethyl)-2-oxopyrrolidin-1-yl]-2H-pyrido[3,2-b][1,4]oxazin-3(4H)-one (Reference Examples 54, 0.11 g, 0.45 mmol), molecular sieve (4 A, 0.1 g) and methanol (4 ml). The obtained mixture was stirred for 20 minutes, cooled on ice and sodium triacetoxyborohydride (0.11 g, 0.58 mmol) was gradually added thereto. Then, the mixture was stirred at room temperature for 4 hours, an aqueous solution of sodium hydrogen carbonate was added thereto and the mixture was extracted with ethyl acetate. The obtained crude product was purified by silica gel column chromatography (dichloromethane/methanol) to yield 15 mg (7%) of the title compound.

後処理

  1. additionwas gradually added
  2. stirringThen, the mixture was stirred at room temperature for 4 hours
  3. extractionthe mixture was extracted with ethyl acetate
  4. customThe obtained crude product
  5. customwas purified by silica gel column chromatography (dichloromethane/methanol)

出典と根拠

ORDレコード
ord-3f33af627a7846b1871241ec3d4d3922
出典データセット
uspto-grants-2015_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08952010B2

反応ノート

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