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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Sodium Hydroxide → tert-butyl (2,3-dihydro(1,4)dioxino(2,3-c)pyridin-7-ylmethyl)(1-(2-(7-fluoro-2-oxo-1,5-naphthyridin-1(2H)-yl)ethyl)piperidin-4-yl)carbamate

HRID 1804729
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HRID 1804729 반응식
O.[O:2]1[C:11]2[CH:10]=[C:9]([CH2:12][N:13]([CH:21]3[CH2:26][CH2:25][NH:24][CH2:23][CH2:22]3)[C:14](=[O:20])[O:15][C:16]([CH3:19])([CH3:18])[CH3:17])[N:8]=[CH:7][C:6]=2[O:5][CH2:4][CH2:3]1.O.Cl.[F:29][C:30]1[CH:39]=[C:38]2[C:33]([CH:34]=[CH:35][C:36](=[O:43])[N:37]2[CH2:40][CH:41]=O)=[N:32][CH:31]=1.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].[OH-].[Na+]>CN1CCCC1=O.O>[O:2]1[C:11]2[CH:10]=[C:9]([CH2:12][N:13]([CH:21]3[CH2:26][CH2:25][N:24]([CH2:41][CH2:40][N:37]4[C:38]5[C:33](=[N:32][CH:31]=[C:30]([F:29])[CH:39]=5)[CH:34]=[CH:35][C:36]4=[O:43])[CH2:23][CH2:22]3)[C:14](=[O:20])[O:15][C:16]([CH3:19])([CH3:18])[CH3:17])[N:8]=[CH:7][C:6]=2[O:5][CH2:4][CH2:3]1
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참가 물질

7

반응물 4

HCID 14798Sodium HydroxideHCID 5049666Sodium triacetoxyborohydrideHCID 86646181(7-fluoro-2-oxo-1,5-naphthyridin-1(2H)-yl)acetaldehyde hydrochloride monohydrateHCID 86646182Tert-butyl (2,3-dihydro(1,4)dioxino(2,3-c)pyridin-7-ylmethyl)(piperidin-4-yl)carbamate monohydrate

생성물 1

HCID 57815262
tert-butyl (2,3-dihydro(1,4)dioxino(2,3-c)pyridin-7-ylmethyl)(1-(2-(7-fluoro-2-oxo-1,5-naphthyridin-1(2H)-yl)ethyl)piperidin-4-yl)carbamate
수율 89.7%

시약·촉매·용매 2

HCID 962Water용매HCID 13387N-methyl-2-pyrrolidone용매2회

실험 절차

To a solution of 5.0 g of tert-butyl (2,3-dihydro(1,4)dioxino(2,3-c)pyridin-7-ylmethyl)(piperidin-4-yl)carbamate monohydrate in 40 mL of N-methyl-2-pyrrolidone, 3.5 g of (7-fluoro-2-oxo-1,5-naphthyridin-1(2H)-yl)acetaldehyde hydrochloride monohydrate was added, and the mixture was stirred for 1 hour at room temperature. To the mixture, 4.3 g of sodium triacetoxyborohydride was added dividedly in 5 portions over the period of 80 minutes under ice cooling, and the mixture was stirred for 1 hour and 40 minutes under ice cooling. After heating to room temperature, the mixture was added with 20 mL of water and adjusted to pH 11.5 with an aqueous solution of 20% sodium hydroxide. To the mixture, 20 mL of N-methyl-2-pyrrolidone was added at 70 to 80° C., and the mixture was stirred for 2 hours and 30 minutes at the same temperature. The reaction mixture was cooled to room temperature and the solid product was obtained by filtration and washed with water to give 6.5 g of tert-butyl (2,3-dihydro(1,4)dioxino(2,3-c)pyridin-7-ylmethyl)(1-(2-(7-fluoro-2-oxo-1,5-naphthyridin-1(2H)-yl)ethyl)piperidin-4-yl)carbamate as a light brown solid.

후처리

  1. stirringthe mixture was stirred for 1 hour and 40 minutes under ice cooling
  2. temperatureAfter heating to room temperature
  3. stirringthe mixture was stirred for 2 hours and 30 minutes at the same temperature
  4. temperatureThe reaction mixture was cooled to room temperature
  5. customthe solid product was obtained by filtration
  6. washwashed with water

출처 및 근거

ORD 기록
ord-2a96420c4889488391cd8081af700cf7
출처 데이터셋
uspto-grants-2013_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08354426B2

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