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Hydrochloric Acid → 2-amino-4-piperazino-7,8-dihydro-6H-thiopyrano[3,2-d]pyrimidine

HRID 1903299
ノート
印刷プレビュー

反応式

HRID 1903299 の反応式
[NH2:1][C:2]1[N:3]=[C:4](Cl)[C:5]2[S:11][CH2:10][CH2:9][CH2:8][C:6]=2[N:7]=1.[NH:13]1[CH2:18][CH2:17][NH:16][CH2:15][CH2:14]1.Cl>C1C=CC=CC=1.CO>[NH2:1][C:2]1[N:3]=[C:4]([N:13]2[CH2:18][CH2:17][NH:16][CH2:15][CH2:14]2)[C:5]2[S:11][CH2:10][CH2:9][CH2:8][C:6]=2[N:7]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 313Hydrochloric Acid2 回HCID 4837PiperazineHCID 133071552-amino-4-chloro-7,8-dihydro-6H-thiopyrano[3,2-d]pyrimidine

生成物 1

HCID 100835282-amino-4-piperazino-7,8-dihydro-6H-thiopyrano[3,2-d]pyrimidine収率 80.2%

試薬・触媒・溶媒 2

HCID 241Benzene溶媒
HCID 887
Methanol
溶媒

実験手順

11 g of 2-amino-4-chloro-7,8-dihydro-6H-thiopyrano[3,2-d]pyrimidine was dissolved in 150 ml of benzene and 30 g of anhydrous piperazine was added thereto while hot. After heating for 3 hours, the mixture was concentrated under reduced pressure and water was added thereto. The mixture was rendered alkaline with potassium carbonate and extracted with chloroform. The organic layer was dried over magnesium sulfate and the solvent was distilled off to obtain crystals. The resulting crystals were converted into the corresponding hydrochloride in methanol and, after treatment with activated carbon, the hydrochloride was again converted into a free base form. The free base was recrystallized from a mixture of chloroform and diethyl ether to obtain 11 g of 2-amino-4-piperazino-7,8-dihydro-6H-thiopyrano[3,2-d]pyrimidine as colorless needles having a melting point of 176°-178° C.

後処理

  1. temperatureAfter heating for 3 hours
  2. concentrationthe mixture was concentrated under reduced pressure and water
  3. additionwas added
  4. extractionextracted with chloroform
  5. dry with materialThe organic layer was dried over magnesium sulfate
  6. distillationthe solvent was distilled off
  7. customto obtain crystals
  8. customThe free base was recrystallized from a mixture of chloroform and diethyl ether

出典と根拠

ORDレコード
ord-95af398cc8ad4df9ad06f88b23897e66
出典データセット
uspto-grants-1984_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04435566

反応ノート

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