Triethylamine → HCID 21285061、化合物

HRID 365223

反応式

HRID 365223 の反応式
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

参加物

7

反応物 4

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

生成物 1

HCID 21285061HCID 21285061、化合物

試薬・触媒・溶媒 2

HCID 6342Acetonitrile溶媒HCID 6344Dichloromethane溶媒

反応条件

温度
80 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-5c50afd2ec26496c93a45e7a11300628
出典データセット
uspto-grants-1986_08
特許番号
US04608373

関連ノート

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