Dichloromethane → HCID 22119844, 화합물

HRID 1274650

반응식

HRID 1274650 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

HCID 22119844HCID 22119844, 화합물

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-ddb3fbe77182416c926ff1265cfa9adf
출처 데이터셋
uspto-grants-2000_12
특허 번호
US06156700

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