Thiomorpholine → 4-[[(4-Thiomorpholinyl)methylene]amino]-3-pyridinol

HRID 362197

반응식

HRID 362197 반응식
[CH3:1][N:2]([CH:4]=[N:5][C:6]1[CH:11]=[CH:10][N:9]=[CH:8][C:7]=1[OH:12])[CH3:3].N1C[CH2:17][S:16][CH2:15]C1>C1(C)C=CC=CC=1>[N:2]1([CH:4]=[N:5][C:6]2[CH:11]=[CH:10][N:9]=[CH:8][C:7]=2[OH:12])[CH2:1][CH2:17][S:16][CH2:15][CH2:3]1

참가 물질

4

반응물 2

HCID 67164ThiomorpholineHCID 153809294-[[(Dimethylamino)methylene]amino]-3-pyridinol

생성물 1

HCID 153809384-[[(4-Thiomorpholinyl)methylene]amino]-3-pyridinol

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

A mixture prepared from 4-[[(dimethylamino)methylene]amino]-3-pyridinol (5.14 g), thiomorpholine (10.5 ml, distilled from CaH2) and dry toluene (120 ml) was refluxed overnight. The reaction mixture was concentrated, triturated with diethyl ether, adhered to silica (methanol), flash chromatographed (10% methanol/ethyl acetate), and triturated with diethyl ether to yield 6.06 g of product. A 3.5 g sample was recrystallized from methanol, and dried under high vacuum and refluxing isopropanol to yield 2.13 g of crystals, m.p. 197°-198.5° C.

후처리

  1. temperaturewas refluxed overnight
  2. concentrationThe reaction mixture was concentrated
  3. customtriturated with diethyl ether
  4. customchromatographed (10% methanol/ethyl acetate)
  5. customtriturated with diethyl ether

출처 및 근거

ORD 기록
ord-291c42efa7ff47deaf37615e4e62ac96
출처 데이터셋
uspto-grants-1999_02
특허 번호
US05869480

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