1,2,3,6-Tetrahydropyridine → 2-methoxyethyl 2-amino-6-[3,6-dihydro-1(2H)-pyridyl]-4-pyrimidinecarbamate

HRID 27232ノート

反応式

HRID 27232 の反応式
[NH2:1][C:2]1[N+:7]([O-])=[C:6]([NH:9][C:10]([O:12][CH2:13][CH2:14][O:15][CH3:16])=[O:11])[CH:5]=[C:4](Cl)[N:3]=1.[NH:18]1[CH2:23][CH2:22][CH:21]=[CH:20][CH2:19]1>C(Cl)(Cl)Cl>[NH2:1][C:2]1[N:7]=[C:6]([NH:9][C:10]([O:12][CH2:13][CH2:14][O:15][CH3:16])=[O:11])[CH:5]=[C:4]([N:18]2[CH2:19][CH:20]=[CH:21][CH2:22][CH2:23]2)[N:3]=1

参加物

4

反応物 2

HCID 127501,2,3,6-TetrahydropyridineHCID 178496340HCID 178496340、化合物

生成物 1

HCID 202857752-methoxyethyl 2-amino-6-[3,6-dihydro-1(2H)-pyridyl]-4-pyrimidinecarbamate

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

反応条件

温度
45 °C

実験手順

2.5 G. of 2-methoxyethyl 2-amino-6-chloro-4-pyrimidinecarbamate-3-oxide are mixed under argon with 3 ml. of 1,2,5,6-tetrahydropyridine and 25 ml. of chloroform. The mixture is stirred at 45° C. for 12 hours, then cooled and washed with 15 ml. of water. The product is extracted with chloroform, the organic phase is dried over sodium sulfate and the solvent is distilled off under reduced pressure. The residue obtained is crystallized from methylene chloride/ether, there being obtained pure 2-methoxyethyl 2-amino-6-[3,6-dihydro-1(2H)-pyridyl]-4-pyrimidinecarbamate having a melting point of 136° C.

後処理

  1. temperaturecooled
  2. washwashed with 15 ml
  3. extractionThe product is extracted with chloroform
  4. dry with materialthe organic phase is dried over sodium sulfate
  5. distillationthe solvent is distilled off under reduced pressure
  6. customThe residue obtained
  7. customis crystallized from methylene chloride/ether, there

出典と根拠

ORDレコード
ord-0b729c248c43465bb70369dea04a29fa
出典データセット
uspto-grants-1980_09
特許番号
US04220772

反応ノート

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