홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

Sodium Carbonate → HCID 21713907, 화합물

HRID 649808
노트
인쇄 미리보기

반응식

HRID 649808 반응식
[CH:1]([CH2:3][N:4]([C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][N:14]=1)[C:5]([CH:7]1[CH2:12][CH2:11][CH2:10][CH2:9][CH2:8]1)=[O:6])=O.[F:19][C:20]([F:35])([F:34])[O:21][C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][C:23]=1[N:28]1[CH2:33][CH2:32][NH:31][CH2:30][CH2:29]1.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].C([O-])([O-])=O.[Na+].[Na+]>O.ClCCCl.C(O)(=O)C>[CH:7]1([C:5]([N:4]([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][N:14]=2)[CH2:3][CH2:1][N:31]2[CH2:30][CH2:29][N:28]([C:23]3[CH:24]=[CH:25][CH:26]=[CH:27][C:22]=3[O:21][C:20]([F:34])([F:19])[F:35])[CH2:33][CH2:32]2)=[O:6])[CH2:12][CH2:11][CH2:10][CH2:9][CH2:8]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 10340Sodium CarbonateHCID 5049666Sodium triacetoxyborohydrideHCID 107529251-(2-Trifluoromethoxyphenyl)piperazineHCID 21713921N-Formylmethyl-N-(2-pyridyl)cyclohexanecarboxamide

생성물 1

HCID 21713907HCID 21713907, 화합물수율 51.1%

시약·촉매·용매 3

HCID 11
1,2-Dichloroethane
용매
HCID 176Acetic Acid용매
HCID 962Water용매

실험 절차

A mixture comprising 0.459 g of Compound 1B, 0.445 g of 1-(2-trifluoromethoxyphenyl)piperaine (prepared as described by D. Clarke et al, in European Patent EP 711 757, 1996), 0.634 g sodium triacetoxyborohydride, 0.23 mL of glacial acetic acid and 15 mL of 1,2-dichloroethane was stirred for 4 h, under a nitrogen atmosphere. The resultant solution was then kept overnight at room temperature, followed by the addition of 10 mL of water, and alkalinization with a 20% aqueous Na2CO3 solution. This was followed by separation of phases, with the isolated aqueous phase being extracted with 2×20 mL dichloromethane, and with the collected organic phases being dried over anhydrous sodium sulphate. This was followed by the removal of solvents, via vacuum evaporation to dryness. The obtained product residue was purified by flash chromatography (ethyl acetate—petroleum ether gradient 90:10 to 10:0). This was followed by evaporation of the solvents, affording 0.44 g of the title compound (yield 51%).

후처리

  1. customThis was followed by separation of phases, with the isolated aqueous phase
  2. extractionbeing extracted with 2×20 mL dichloromethane
  3. dry with materialwith the collected organic phases being dried over anhydrous sodium sulphate
  4. customThis was followed by the removal of solvents, via vacuum evaporation to dryness
  5. customThe obtained product residue was purified by flash chromatography (ethyl acetate—petroleum ether gradient 90:10 to 10:0)
  6. customThis was followed by evaporation of the solvents

출처 및 근거

ORD 기록
ord-0a90b7411b3c4eba8be42f1ec1927717
출처 데이터셋
uspto-grants-2001_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06271234B1

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트