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

Dimethylformamide → HCID 178457084, 화합물

HRID 1443834
노트
인쇄 미리보기

반응식

HRID 1443834 반응식
C([O:8][C:9]1[CH:17]=[C:16]([O:18]CC2C=CC=CC=2)[C:15]([CH:26]([CH3:28])[CH3:27])=[CH:14][C:10]=1[C:11](O)=O)C1C=CC=CC=1.C(Cl)(=O)C(Cl)=O.C[N:36]([CH:38]=[O:39])C.[CH3:40][O:41][C:42]1[CH:47]=[CH:46][C:45]([NH2:48])=[CH:44][C:43]=1[N:49]([CH3:53])[CH2:50][CH2:51][CH3:52].C([N:56](CC)CC)C>ClCCl.C1COCC1.O.C(OCC)(=O)C>[OH:39][C:38]1[N:48]([C:45]2[CH:46]=[CH:47][C:42]([O:41][CH3:40])=[C:43]([N:49]([CH3:53])[CH2:50][CH2:51][CH3:52])[CH:44]=2)[C:11]([C:10]2[CH:14]=[C:15]([CH:26]([CH3:27])[CH3:28])[C:16]([OH:18])=[CH:17][C:9]=2[OH:8])=[N:56][N:36]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

10

반응물 5

HCID 6228DimethylformamideHCID 8471TriethylamineHCID 65578Oxalyl chlorideHCID 591678792,4-Dibenzyloxy-5-isopropyl-benzoic acidHCID 591678804-Methoxy-N3-methyl-N3-propyl-benzene-1,3-diamine

생성물 1

HCID 178457084HCID 178457084, 화합물수율 93%

시약·촉매·용매

4
HCID 962Water용매HCID 6344Dichloromethane용매HCID 8028Tetrahydrofuran용매2회HCID 8857Ethyl Acetate용매

실험 절차

2,4-Bis-benzyloxy-5-isopropylbenzoic acid (1.25 g, 3.32 mmol) was dissolved in dichloromethane (50 mL) and cooled in an ice bath. Oxalyl chloride (0.32 mL, 3.65 mmol) was added followed by the dropwise addition of DMF (0.1 mL). The reaction was stirred at room temperature for 1 hr then evaporated to dryness under reduced pressure to produce a brown solid. This solid was dissolved in THF (50 mL) and cooled in an ice bath. A solution of 4-Methoxy-N3-methyl-N3-propyl-benzene-1,3-diamine (0.71 g, 3.65 mmol) in THF (20 mL) was added dropwisely followed by the triethylamine (1.6 mL) and the reaction was stirred at room temperature for 16 hrs. Ethyl acetate (50 mL) and water (100 mL) were added. The ethyl acetate layer was washed with water (3×50 mL), dried over magnesium sulfate, filtered and evaporated to dryness to produce the crude product as a brown solid. Purification by silicagel chromatography (elution with 25% ethyl acetate/hexane) provided the desired compound as a white solid (1.8 g, 93%).

후처리

  1. temperaturecooled in an ice bath
  2. customthen evaporated to dryness under reduced pressure
  3. customto produce a brown solid
  4. temperaturecooled in an ice bath
  5. stirringthe reaction was stirred at room temperature for 16 hrs
  6. washThe ethyl acetate layer was washed with water (3×50 mL)
  7. dry with materialdried over magnesium sulfate
  8. filtrationfiltered
  9. customevaporated to dryness
  10. customto produce the crude product as a brown solid
  11. customPurification
  12. washby silicagel chromatography (elution with 25% ethyl acetate/hexane)

출처 및 근거

ORD 기록
ord-11a2111d891840a58e80d7338b703ffc
출처 데이터셋
uspto-grants-2010_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07662813B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트