ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
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
  1. ホーム
  2. /反応

Acetic Acid → {2-[5-(1-Methyl-2-oxo-1,2,3,4-tetrahydro-quinolin-6-yl)-3,4-dihydro-2H-[1,7]naphthyridin-1-yl]-ethyl}-carbamic acid tert-butyl ester

HRID 530351
ノート
印刷プレビュー

反応式

HRID 530351 の反応式
[CH3:1][N:2]1[C:11]2[C:6](=[CH:7][C:8]([C:12]3[CH:21]=[N:20][CH:19]=[C:18]4[C:13]=3[CH2:14][CH2:15][CH2:16][NH:17]4)=[CH:9][CH:10]=2)[CH2:5][CH2:4][C:3]1=[O:22].O=[CH:24][CH2:25][NH:26][C:27](=[O:33])[O:28][C:29]([CH3:32])([CH3:31])[CH3:30].C(O)(=O)C.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].C([O-])(O)=O.[Na+]>ClCCCl.C(Cl)Cl.C1COCC1>[C:29]([O:28][C:27](=[O:33])[NH:26][CH2:25][CH2:24][N:17]1[C:18]2[C:13](=[C:12]([C:8]3[CH:7]=[C:6]4[C:11](=[CH:10][CH:9]=3)[N:2]([CH3:1])[C:3](=[O:22])[CH2:4][CH2:5]4)[CH:21]=[N:20][CH:19]=2)[CH2:14][CH2:15][CH2:16]1)([CH3:32])([CH3:31])[CH3:30]
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 5

HCID 176Acetic AcidHCID 516892Sodium BicarbonateHCID 4247255tert-butyl N-(2-oxoethyl)carbamateHCID 5049666Sodium triacetoxyborohydrideHCID 866799281-Methyl-6-(1,2,3,4-tetrahydro-1,7-naphthyridin-5-yl)-3,4-dihydroquinolin-2(1H)-one

生成物 1

HCID 71536484
{2-[5-(1-Methyl-2-oxo-1,2,3,4-tetrahydro-quinolin-6-yl)-3,4-dihydro-2H-[1,7]naphthyridin-1-yl]-ethyl}-carbamic acid tert-butyl ester
収率 24.2%

試薬・触媒・溶媒 3

HCID 111,2-Dichloroethane溶媒HCID 6344Dichloromethane溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of 1-methyl-6-(1,2,3,4-tetrahydro-1,7-naphthyridin-5-yl)-3,4-dihydroquinolin-2(1H)-one (intermediate A-5, 0.1 g, 0.341 mmol) in DCE (3 mL)/THF (1.5 mL) were added tert-butyl 2-oxoethylcarbamate (0.081 g, 0.511 mmol), acetic acid (0.02 g, 0.341 mmol) and the reaction mixture was stirred at room temperature for 10 min. Then, sodium triacetoxyborohydride (0.144 g, 0.682 mmol) was added and stirring was continued at room temperature over night. Then, the mixture was diluted with DCM, poured into aq NaHCO3 and extracted with DCM (2×25 mL). Combined organics were washed with brine, dried over Na2SO4, filtered and evaporated to dryness. The residue was purified by reverse phase HPLC on a Gemini-NX column, eluting with a 20 to 98% MeOH—H2O (0.05% TEA) gradient to give the title compound (0.036 g, 24%) as a white foam. MS: 437.2 (M+H+).

後処理

  1. stirringstirring
  2. waitwas continued at room temperature over night
  3. extractionextracted with DCM (2×25 mL)
  4. washCombined organics were washed with brine
  5. dry with materialdried over Na2SO4
  6. filtrationfiltered
  7. customevaporated to dryness
  8. customThe residue was purified by reverse phase HPLC on a Gemini-NX column
  9. washeluting with a 20 to 98% MeOH—H2O (0.05% TEA) gradient

出典と根拠

ORDレコード
ord-46c75fa127ee4202ba645e255413c4dd
出典データセット
uspto-grants-2016_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09353081B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート