Dichloromethane → HCID 22119844、化合物

HRID 1274650

反応式

HRID 1274650 の反応式
[OH:1][CH2:2][C:3]1[C:7]2[CH:8]=[C:9]([N:12]3[C:17](=[O:18])[CH:16]=[C:15]([C:19]([F:22])([F:21])[F:20])[N:14]([CH3:23])[C:13]3=[O:24])[CH:10]=[CH:11][C:6]=2[S:5][N:4]=1.C(Cl)Cl.C(N(C(C)C)C(C)C)C.[CH2:37]([O:39][CH2:40]Cl)[CH3:38]>CCOCC>[CH2:37]([O:39][CH2:40][O:1][CH2:2][C:3]1[C:7]2[CH:8]=[C:9]([N:12]3[C:17](=[O:18])[CH:16]=[C:15]([C:19]([F:21])([F:20])[F:22])[N:14]([CH3:23])[C:13]3=[O:24])[CH:10]=[CH:11][C:6]=2[S:5][N:4]=1)[CH3:38]

参加物

6

反応物 4

HCID 6344DichloromethaneHCID 18523Chloromethyl ethyl etherHCID 81531DiisopropylethylamineHCID 221198213-[3-(hydroxymethyl)-1,2-benzisothiazol-5-yl]-1-methyl-6-(trifluoromethyl)-2,4(1H,3H)-pyrimidinedione

生成物 1

HCID 22119844HCID 22119844、化合物

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

To a mixture of 3-[3-(hydroxymethyl)-1,2-benzisothiazol-5-yl]-1-methyl-6-(trifluoromethyl)-2,4(1H,3H)-pyrimidinedione (0.800 g, 0.00224 mol) and methylene chloride is added ethyldiisopropylamine (0.780 ml, 0.00448 mol) followed by chloromethyl ethyl ether (0.310 ml, 0.00336 mol). The resultant mixture is stirred 42.5 hours at room temperature, diluted with ether, washed sequentially with 1 M aqueous hydrochloric acid, saturated sodium bicarbonate and brine, dried over anhydrous magnesium sulfate, filtered, and concentrated in vacuo to a yellow syrup. The syrup is chromatographed on silica gel with hexanes:ethyl acetate to give the product as a white solid which is identified by NMR spectral analysis.

後処理

  1. washwashed sequentially with 1 M aqueous hydrochloric acid, saturated sodium bicarbonate and brine
  2. dry with materialdried over anhydrous magnesium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated in vacuo to a yellow syrup
  5. customThe syrup is chromatographed on silica gel with hexanes

出典と根拠

ORDレコード
ord-ddb3fbe77182416c926ff1265cfa9adf
出典データセット
uspto-grants-2000_12
特許番号
US06156700

関連ノート

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