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

1,2-Dichloroethane → HCID 54591523, 화합물

HRID 1260201
노트
인쇄 미리보기

반응식

HRID 1260201 반응식
C(Cl)CCl.[CH3:5][C:6]1[N:10]([CH2:11][C:12]2[CH:13]=[C:14]([N:18]3[CH2:21][CH:20]([OH:22])[CH2:19]3)[CH:15]=[CH:16][CH:17]=2)[N:9]=[C:8]([C:23]2[O:27][N:26]=[C:25]([C:28]3[CH:33]=[CH:32][C:31]([O:34][C:35]([F:38])([F:37])[F:36])=[CH:30][CH:29]=3)[N:24]=2)[CH:7]=1.[CH3:39][N:40]([CH3:45])[CH2:41][C:42](O)=[O:43]>ClCCl.C(OCC)(=O)C>[CH3:39][N:40]([CH3:45])[CH2:41][C:42]([O:22][CH:20]1[CH2:21][N:18]([C:14]2[CH:15]=[CH:16][CH:17]=[C:12]([CH2:11][N:10]3[C:6]([CH3:5])=[CH:7][C:8]([C:23]4[O:27][N:26]=[C:25]([C:28]5[CH:33]=[CH:32][C:31]([O:34][C:35]([F:38])([F:36])[F:37])=[CH:30][CH:29]=5)[N:24]=4)=[N:9]3)[CH:13]=2)[CH2:19]1)=[O:43]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 111,2-DichloroethaneHCID 673N,N-DimethylglycineHCID 54591302HCID 54591302, 화합물

생성물 1

HCID 54591523HCID 54591523, 화합물수율 50.4%

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 8857Ethyl Acetate용매

실험 절차

86 mg (0.70 mmol) of 4-N,N-dimethylaminopyridine and 671 mg (3.50 mmol) of EDC were added to a solution of 550 mg (1.17 mmol) of the compound from Example 1 and 361 mg (3.50 mmol) of N,N-dimethylglycine in 11 ml of dichloromethane. After the reaction mixture had been stirred at RT for 8 h, all volatile constituents were removed on a rotary evaporator. The residue obtained was taken up in 200 ml of ethyl acetate and washed once with approx. 100 ml of water. After drying over anhydrous magnesium sulphate, filtration and concentration, the product was isolated by means of MPLC (approx. 30 g of silica gel, eluent: 25:25:1 cyclohexane/ethyl acetate/triethylamine) A first fraction of 328 mg of the title compound was obtained. A further 115 mg of the title compound were obtained from a second, still-contaminated fraction by recrystallization from cyclopentyl methyl ether. A total of 443 mg (68% of theory) of the title compound was thus obtained. Another crystallization from diisopropyl ether/cyclopentyl methyl ether (2:1, 1.5 ml per 100 mg) gave the title compound with a melting point of 117° C.

후처리

  1. customall volatile constituents were removed on a rotary evaporator
  2. customThe residue obtained
  3. washwashed once with approx. 100 ml of water
  4. dry with materialAfter drying over anhydrous magnesium sulphate, filtration and concentration

출처 및 근거

ORD 기록
ord-55a706e153b442b4979bc9dc79e6420a
출처 데이터셋
uspto-grants-2013_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08470811B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트