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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Sodium Hydroxide → HCID 66680556, 화합물

HRID 1966965
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HRID 1966965 반응식
[OH-].[Na+].C([O:5][C:6](=[O:27])[CH2:7][N:8]1[C:12](=[O:13])[C:11]2([CH2:18][CH2:17][CH2:16][CH2:15][CH2:14]2)[N:10]([C:19]2[CH:24]=[CH:23][C:22]([CH3:25])=[CH:21][CH:20]=2)[C:9]1=[O:26])C>C1COCC1>[O:26]=[C:9]1[N:8]([CH2:7][C:6]([OH:27])=[O:5])[C:12](=[O:13])[C:11]2([CH2:14][CH2:15][CH2:16][CH2:17][CH2:18]2)[N:10]1[C:19]1[CH:20]=[CH:21][C:22]([CH3:25])=[CH:23][CH:24]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 66679752HCID 66679752, 화합물

생성물 1

HCID 66680556HCID 66680556, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

172 ml (0.172 mol; 1.5 eq.) of 1N sodium hydroxide are added to a solution of 39.5 g (0.114 mol; 1 eq.) of (2,4-dioxo-1-p-tolyl-1,3-diazaspiro[4.5]dec-3-yl)acetic acid ethyl ester in 400 ml of THF. The reaction medium is stirred at room temperature for about 72 hours. The reaction medium is concentrated and 250 ml of ethyl acetate are added, followed by 400 ml of water. 100 ml of 1N NaOH are added and the aqueous solution is washed with 250 ml of ethyl acetate. The aqueous phase is concentrated and then acidified to pH 4 approximately with 170 ml of 1N acetic acid. The white precipitate is filtered off and then rinsed with water until the pH of the filtrates is approximately equal to 7, and dried in an oven under vacuum at 40° C. The product (2,4-dioxo-1-p-tolyl-1,3-diazaspiro[4.5]dec-3-yl)acetic acid is obtained in the form of a white solid.

후처리

  1. concentrationThe reaction medium is concentrated
  2. addition250 ml of ethyl acetate are added
  3. addition100 ml of 1N NaOH are added
  4. washthe aqueous solution is washed with 250 ml of ethyl acetate
  5. concentrationThe aqueous phase is concentrated
  6. filtrationThe white precipitate is filtered off
  7. washrinsed with water until the pH of the filtrates
  8. customdried in an oven under vacuum at 40° C

출처 및 근거

ORD 기록
ord-32559c43b1d041f9baa72d9c71be477a
출처 데이터셋
uspto-grants-2013_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08420681B2

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