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Hydrazine hydrate (1:1) → HCID 20094178、化合物

HRID 273782
ノート
印刷プレビュー

反応式

HRID 273782 の反応式
Cl[C:2]1[C:3]2[S:12][CH:11]=[CH:10][C:4]=2[N:5]=[C:6]([CH2:8][Cl:9])[N:7]=1.O.[NH2:14][NH2:15]>O1CCCC1>[Cl:9][CH2:8][C:6]1[N:7]=[C:2]([NH:14][NH2:15])[C:3]2[S:12][CH:11]=[CH:10][C:4]=2[N:5]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 200941424-Chloro-2-(chloromethyl)thieno[3,2-d]pyrimidine

生成物 1

HCID 20094178HCID 20094178、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
5 °C

実験手順

3. 8.2 g of 4-chloro-2-(chloromethyl)thieno[3,2-d]pyrimidine are dissolved in 500 ml of absolute tetrahydrofuran. The solution is cooled to 5° C. 7 ml of hydrazine hydrate are added dropwise within 5 min., whereby a solution results and the temperature rises to 15° to 20° C. The reaction mixture is stirred at room temperature for 15 h. and then evaporated in a vacuum. The residue is stirred with 100 ml of saturated aqueous sodium hydrogen carbonate solution for 30 min. and then filtered off. The crystals are washed neutral with water and dried in a vacuum. 14.7 g of 2-(chloromethyl)-4-hydrazinothieno[3,2-d]-pyrimidine are obtained. A further 1.0 g of 2-(chloromethyl)-4-hydrazinothieno[3,2-d]pyrimidine are obtained by extracting the filtrate with chloroform.

後処理

  1. customwhereby a solution results
  2. customrises to 15° to 20° C
  3. customevaporated in a vacuum
  4. stirringThe residue is stirred with 100 ml of saturated aqueous sodium hydrogen carbonate solution for 30 min.
  5. filtrationfiltered off
  6. washThe crystals are washed neutral with water
  7. customdried in a vacuum

出典と根拠

ORDレコード
ord-911d0d7334fb464b8e4f979a0f0487a8
出典データセット
uspto-grants-1995_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05387585

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート