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

HRID 361330

反応式

HRID 361330 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-2bc39261f74746edae224d78ee97c69e
出典データセット
uspto-grants-1999_02
特許番号
US05866565

関連ノート

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