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

HRID 361330

반응식

HRID 361330 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-2bc39261f74746edae224d78ee97c69e
출처 데이터셋
uspto-grants-1999_02
특허 번호
US05866565

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