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Hydrazine hydrate (1:1) → HCID 20094178, 화합물

HRID 273782
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HRID 273782 반응식
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
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참가 물질

4

반응물 2

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

생성물 1

HCID 20094178HCID 20094178, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
5 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-911d0d7334fb464b8e4f979a0f0487a8
출처 데이터셋
uspto-grants-1995_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05387585

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