Potassium Carbonate → HCID 12942564, 화합물

HRID 2198411노트

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HRID 2198411 반응식
[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[N:7]1[CH:11]=[N:10][C:9]([OH:12])=[N:8]1.C(=O)([O-])[O-].[K+].[K+].[P:19](=[S:25])(Cl)([O:22][CH3:23])[O:20][CH3:21]>C(#N)C.CN(C)C1C=CN=CC=1>[P:19](=[S:25])([O:12][C:9]1[N:10]=[CH:11][N:7]([C:2]2[CH:3]=[CH:4][CH:5]=[CH:6][N:1]=2)[N:8]=1)([O:22][CH3:23])[O:20][CH3:21]

참가 물질

6

반응물 3

HCID 11430Potassium CarbonateHCID 17304Dimethyl phosphorochloridothionateHCID 178518009HCID 178518009, 화합물

생성물 1

HCID 12942564HCID 12942564, 화합물

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 6342Acetonitrile용매3회

실험 절차

A mixture of 8.10 g (0.05 m) of 1-(2-pyridinyl)-1H-1,2,4-triazol-3-ol and 8.29 g (0.06 m) of powdered potassium carbonate in 150 ml of acetonitrile was vigorously stirred together for 21/2 hours at 40°-50° C. To this mixture was successively added a solution of 0.29 g (0.0024 m (5 mole percent)) of 4-dimethylaminopyridine in 25 ml of acetonitrile followed by a solution of 7.94 g (0.048 m) of O,O-dimethyl phosphorochloridothioate in 25 ml of acetonitrile. After a 2 hour period, the reaction was complete and the reaction mixture was filtered and evaporated to dryness. The oil which remained as a residue was triturated with hexane and solidification occurred. The solid, crude O,O-dimethyl O-(1-(2-pyridinyl)-1H-1,2,4-triazol-3-yl) phosphorothioate product was recovered in a yield of 11.3 g (82 percent of theoretical) and melted at 88°-91° C. The product after recrystallization from methyl cyclohexane melted at 95°-96° C. Upon analysis, the product was found to have carbon, hydrogen and nitrogen contents of 37.68, 3.91 and 19.51 percent, respectively, as compared with the theoretical contents of 37.76, 3.87 and 19.58 percent, respectively, as calculated for the named compound. (Compound 6).

후처리

  1. waitAfter a 2 hour period
  2. filtrationthe reaction mixture was filtered
  3. customevaporated to dryness
  4. customwas triturated with hexane and solidification
  5. customThe solid, crude O,O-dimethyl O-(1-(2-pyridinyl)-1H-1,2,4-triazol-3-yl) phosphorothioate product was recovered in a yield of 11.3 g (82 percent of theoretical) and melted at 88°-91° C
  6. customThe product after recrystallization from methyl cyclohexane melted at 95°-96° C

출처 및 근거

ORD 기록
ord-81332cc775314975b035e482e609e8b5
출처 데이터셋
uspto-grants-1982_11
특허 번호
US04357328

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