Triethylamine → HCID 21285061, 화합물

HRID 365223

반응식

HRID 365223 반응식
O[N:2]1[C:6](=[O:7])[C:5]2=[CH:8][CH:9]=[CH:10][CH:11]=[C:4]2[C:3]1=[O:12].C(N(CC)CC)C.Cl[CH2:21][C:22]1[N:23]=[C:24]([NH:27][C:28]([C:41]2[CH:46]=[CH:45][CH:44]=[CH:43][CH:42]=2)([C:35]2[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=2)[C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=2)[S:25][CH:26]=1.C(OCC)(=[O:49])C>C(#N)C.ClCCl>[C:28]([NH:27][C:24]1[S:25][CH:26]=[C:22]([CH2:21][O:49][C:8]2[CH:9]=[CH:10][CH:11]=[C:4]3[C:3]([NH:2][C:6](=[O:7])[C:5]=23)=[O:12])[N:23]=1)([C:41]1[CH:46]=[CH:45][CH:44]=[CH:43][CH:42]=1)([C:35]1[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=1)[C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1

참가 물질

7

반응물 4

HCID 8471TriethylamineHCID 8857Ethyl AcetateHCID 10665N-HydroxyphthalimideHCID 137451724-Chloromethyl-2-tritylaminothiazole

생성물 1

HCID 21285061HCID 21285061, 화합물

시약·촉매·용매 2

HCID 6342Acetonitrile용매HCID 6344Dichloromethane용매

반응 조건

온도
80 °C

실험 절차

In 150 ml of acetonitrile was suspended 11.48 g of N-hydroxyphthalimide. To the suspension was added 7.11 g of triethylamine and dissoled therein. To the solution was added a solution of 27.5 g of 4-chloromethyl-2-tritylaminothiazole dissolved in 200 ml of dichloromethane and the mixture was stirred on an oil bath of 80° C. for 7 hours. The reaction mixture thus obtained was concentrated and the residue formed was dissolved in ethyl acetate. The solution was washed with water, dried by anhydrous magnesium sulfate, and concentrated. The residue was applied to column chromatography and the product was eluted with chloroform to provide 14.5 g of (2-tritylamino-4-thiazolyl)methoxyphthalimide.

후처리

  1. customThe reaction mixture thus obtained
  2. concentrationwas concentrated
  3. customthe residue formed
  4. washThe solution was washed with water
  5. dry with materialdried by anhydrous magnesium sulfate
  6. concentrationconcentrated
  7. washthe product was eluted with chloroform

출처 및 근거

ORD 기록
ord-5c50afd2ec26496c93a45e7a11300628
출처 데이터셋
uspto-grants-1986_08
특허 번호
US04608373

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