Triethylamine → 1-(Methylthiomethyl)-6-phenylthiothymine

HRID 1057248노트

반응식

HRID 1057248 반응식
Cl[CH2:2][S:3][CH3:4].[C:5]1([C:11]2[NH:16][C:15](=[S:17])[NH:14][C:13](=[O:18])[C:12]=2[CH3:19])[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1.C(N(CC)CC)C>CN(C)C=O>[CH3:4][S:3][CH2:2][N:16]1[C:11]([C:5]2[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=2)=[C:12]([CH3:19])[C:13](=[O:18])[NH:14][C:15]1=[S:17]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 16916Chloromethyl methyl sulfideHCID 186710275-Methyl-6-phenyl-2-sulfanylidene-1,2,3,4-tetrahydropyrimidin-4-one

생성물 1

HCID 538403951-(Methylthiomethyl)-6-phenylthiothymine수율 8.1%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To 4 ml of dimethylformamide, 0.17 ml (2.0 mmol) of chloromethylmethylsulfide, 0.47 g (2.0 mmol) of 6-phenylthiothymine, 0.56 ml (2.0 mmol) of triethylamine were added and allowed to react for 22 hours at room temperature. The reaction mixture was concentrated under reduced pressure and the residue was adsorbed on a silica gel column and eluted with chloroform. The eluate was concentrated and crystallized from ethyl acetate to obtain 45 mg of the target compound (Yield: 8%).

후처리

  1. customto react for 22 hours at room temperature
  2. concentrationThe reaction mixture was concentrated under reduced pressure
  3. washeluted with chloroform
  4. concentrationThe eluate was concentrated
  5. customcrystallized from ethyl acetate

출처 및 근거

ORD 기록
ord-331e78f44cf74847817221983cb31339
출처 데이터셋
uspto-grants-2003_02
특허 번호
USRE037979E1

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