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2-nitromethylenetetrahydro-2H-1,3-thiazine → 2-(5,6-Dihydro-4H-1,3-thiazin-2-yl)-N,N-dimethyl-2-nitroethen-1-amine

HRID 1576496
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HRID 1576496 반응식
[N+:1]([CH:4]=[C:5]1[NH:10][CH2:9][CH2:8][CH2:7][S:6]1)([O-:3])=[O:2].CO[CH:13](OC)[N:14]([CH3:16])[CH3:15]>C(Cl)(Cl)Cl>[S:6]1[CH2:7][CH2:8][CH2:9][N:10]=[C:5]1[C:4]([N+:1]([O-:3])=[O:2])=[CH:13][N:14]([CH3:16])[CH3:15]
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참가 물질

4

반응물 2

HCID 428532-nitromethylenetetrahydro-2H-1,3-thiazineHCID 78373Dimethylformamide dimethyl acetal

생성물 1

HCID 538694182-(5,6-Dihydro-4H-1,3-thiazin-2-yl)-N,N-dimethyl-2-nitroethen-1-amine

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

8.0 G OF TETRAHYDRO-2-(NITROMETHYLENE)-2H-1,3-thiazine, prepared as described in Example 2 of Ser. No. 554,361, 5.95 g of N,N-dimethylformamide dimethyl acetal and 25 ml of chloroform were mixed and the mixture was refluxed for about 16 hours. The solvent then was evaporated under reduced pressure to leave a dark orange solid. Recrystallization from ethyl acetate and methanol gave (1), as a light orange solid, m.p.: 168.5°-170°.

후처리

  1. temperaturethe mixture was refluxed for about 16 hours
  2. customThe solvent then was evaporated under reduced pressure
  3. customto leave a dark orange solid
  4. customRecrystallization from ethyl acetate and methanol

출처 및 근거

ORD 기록
ord-8bb9d52282b845a8a9bd24360ae11130
출처 데이터셋
uspto-grants-1976_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03981871

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