Hydrochloric Acid → Tetrahydro-3-methyl-2-(nitromethylene)-1,3-thiazine

HRID 978605노트

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HRID 978605 반응식
[CH3:1][NH:2][CH2:3][CH2:4][CH2:5][SH:6].[OH-].[Na+].Cl[C:10](Cl)=[CH:11][N+:12]([O-:14])=[O:13].Cl>CO.C(Cl)Cl.O>[CH3:1][N:2]1[CH2:3][CH2:4][CH2:5][S:6][C:10]1=[CH:11][N+:12]([O-:14])=[O:13]

참가 물질

8

반응물 4

HCID 313Hydrochloric AcidHCID 14798Sodium Hydroxide2회HCID 122195711,1-Dichloro-2-nitroetheneHCID 126345101-Methylamino-3-propanethiol

생성물 1

HCID 54288034Tetrahydro-3-methyl-2-(nitromethylene)-1,3-thiazine수율 98.3%

시약·촉매·용매 3

HCID 887Methanol용매3회HCID 962Water용매HCID 6344Dichloromethane용매

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온도
0 °C

실험 절차

Into 40 ml of methanol were added 5.0 g of 1-methylamino-3-propanethiol and 0.8 g of caustic soda, followed by stirring, to be completely dissolved therein. Then, the mixture was cooled to 0° C. While stirring the solution, a solution of 1.6 g of caustic soda dissolved in 25 ml of methanol and a solution of 2.8 g of 2,2-dichloronitroethylene diluted in 20 ml of methanol were added at the same time dropwise slowly over 50 minutes, and the reaction was carried out for one hour at about 8° C. After the reaction, the reaction mixture was neutralized to pH 7 with 3 N aqueous hydrochloric acid, and then with addition of 60 ml of water, extraction with 50 ml of methylene chloride was repeated four times. The extracts were concentrated to give 3.38 g of tetrahydro-3-methyl-2-(nitromethylene)-1,3-thiazine (yield: 97%).

후처리

  1. dissolutionto be completely dissolved
  2. stirringWhile stirring the solution
  3. additionwere added at the same time dropwise slowly over 50 minutes
  4. customAfter the reaction
  5. concentrationThe extracts were concentrated

출처 및 근거

ORD 기록
ord-b92e1cb9685a4fa5a23cdd426fca6e64
출처 데이터셋
uspto-grants-1987_05
특허 번호
US04665172

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