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llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
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Benzoyl chloride → N-{3-[2-(3-Azabicyclo[3.2.2]non-3-yl)ethyl]-1,3,4,5-tetrahydro-8-methyl-5-oxo-2H-[1]benzopyrano[3,4-c]pyridin-9-yl}-benzamide

HRID 1995300
ノート
印刷プレビュー

反応式

HRID 1995300 の反応式
[NH2:1][C:2]1[C:3]([CH3:28])=[CH:4][C:5]2[O:26][C:25](=[O:27])[C:9]3[CH2:10][N:11]([CH2:14][CH2:15][N:16]4[CH2:22][CH:21]5[CH2:23][CH2:24][CH:18]([CH2:19][CH2:20]5)[CH2:17]4)[CH2:12][CH2:13][C:8]=3[C:6]=2[CH:7]=1.C(=O)([O-])[O-].[K+].[K+].[C:35](Cl)(=[O:42])[C:36]1[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=1>C(Cl)(Cl)Cl>[CH:21]12[CH2:23][CH2:24][CH:18]([CH2:19][CH2:20]1)[CH2:17][N:16]([CH2:15][CH2:14][N:11]1[CH2:12][CH2:13][C:8]3[C:6]4[CH:7]=[C:2]([NH:1][C:35](=[O:42])[C:36]5[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=5)[C:3]([CH3:28])=[CH:4][C:5]=4[O:26][C:25](=[O:27])[C:9]=3[CH2:10]1)[CH2:22]2
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 7412Benzoyl chlorideHCID 11430Potassium CarbonateHCID 13189028HCID 13189028、化合物

生成物 1

HCID 13189030N-{3-[2-(3-Azabicyclo[3.2.2]non-3-yl)ethyl]-1,3,4,5-tetrahydro-8-methyl-5-oxo-2H-[1]benzopyrano[3,4-c]pyridin-9-yl}-benzamide収率 38.2%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

A mixture of 9-amino-3-[2-(3-azabicyclo[3.2.2]non-3-yl)ethyl]-1,2,3,4-tetrahydro-8-methyl-5H-benzopyrano[3,4-c]pyridin-5-one (2.5 g, 0.007 moles), potassium carbonate (2.4 g, 0.017 moles), and benzoyl chloride (1.0 ml, 0.009 moles) is stirred in chloroform (50 ml) at room temperature. After 24 hours the mixture is poured into ice water. The layers are separated, and the aqueous phase is extracted with chloroform (2×60 ml). The combined organic extracts are washed with brine and dried (magnesium sulfate). The solvent is removed under reduced pressure to leave a syrup, which crystallized from ethyl acetate. Recrystallization gave the product (1.3 g), mp 174°-176° C.

後処理

  1. customThe layers are separated
  2. extractionthe aqueous phase is extracted with chloroform (2×60 ml)
  3. washThe combined organic extracts are washed with brine
  4. dry with materialdried (magnesium sulfate)
  5. customThe solvent is removed under reduced pressure
  6. customto leave a syrup, which
  7. customcrystallized from ethyl acetate
  8. customRecrystallization

出典と根拠

ORDレコード
ord-611ef74cdcf8443d93117f3e9dbcb7ea
出典データセット
uspto-grants-1983_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04404138

反応ノート

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