Pyridine → Carbamic acid, ((bis(2-cyanoethyl)amino)thio)methyl-, 2,3-dihydro-2,2-dimethyl-7-benzofuranyl ester

HRID 905001

반응식

HRID 905001 반응식
[CH3:1][NH:2][C:3](=[O:16])[O:4][C:5]1[C:13]2[O:12][C:11]([CH3:15])([CH3:14])[CH2:10][C:9]=2[CH:8]=[CH:7][CH:6]=1.[C:17]([CH2:19][CH2:20][N:21]([CH2:24][CH2:25][C:26]#[N:27])[S:22]Cl)#[N:18].N1C=CC=CC=1>C(Cl)Cl>[C:17]([CH2:19][CH2:20][N:21]([CH2:24][CH2:25][C:26]#[N:27])[S:22][N:2]([CH3:1])[C:3](=[O:16])[O:4][C:5]1[C:13]2[O:12][C:11]([CH3:14])([CH3:15])[CH2:10][C:9]=2[CH:8]=[CH:7][CH:6]=1)#[N:18]

참가 물질

5

반응물 3

HCID 1049PyridineHCID 2566CarbofuranHCID 13269371HCID 13269371, 화합물

생성물 1

HCID 3067958Carbamic acid, ((bis(2-cyanoethyl)amino)thio)methyl-, 2,3-dihydro-2,2-dimethyl-7-benzofuranyl ester

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

4.4 g (0.02 mole) of 2,3-dihydro-2,2-dimethylbenzofuran-7-yl N-methyl-carbamate, 3.8 g (0.02 mole) of bis(cyanoethyl)aminosulfenyl chloride obtained in Example 31, and 4.7 g (0.06 mole) of pyridine were dissolved in 35 ml of methylene chloride, and the resulting solution was stirred for 20 hours at 25° to 30° C. After completion of the reaction, the reaction solution was washed successively with water, diluted hydrochloric acid and water. The methylene chloride layer was dried over sodium sulfate and concentrated under reduced pressure to obtain an oily product which was almost entirely composed of the desired product although containing small amounts of the starting materials and impurities. Yield: 6.2 g (82.7%).

후처리

  1. customAfter completion of the reaction
  2. washthe reaction solution was washed successively with water, diluted hydrochloric acid and water
  3. dry with materialThe methylene chloride layer was dried over sodium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customto obtain an oily product which

출처 및 근거

ORD 기록
ord-421fc68e00ae4b268b5a51d22b59f159
출처 데이터셋
uspto-grants-1983_12
특허 번호
US04421693

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