Dibromomethane → 2-(Phenylthiomethylimino)-1,3-dithietane

HRID 1283685노트

반응식

HRID 1283685 반응식
C(Br)Br.[CH2:4](N(CC)CC)C.[C:11]1([S:17][CH2:18][NH:19][C:20](=[S:22])[S-:21])[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1.[K+].S1CCS1>O.CN(C)C=O>[C:11]1([S:17][CH2:18][N:19]=[C:20]2[S:21][CH2:4][S:22]2)[CH:12]=[CH:13][CH:14]=[CH:15][CH:16]=1

참가 물질

7

반응물 4

HCID 3024DibromomethaneHCID 8471TriethylamineHCID 123092831,2-DithietaneHCID 23667329Potassium phenylthiomethyldithiocarbamate

생성물 1

HCID 214533212-(Phenylthiomethylimino)-1,3-dithietane

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

To a mixture of 28.2 g. of methylene bromide and 10.9 g. of triethylamine in 250 ml. of dimethylformamide was added, in portions, 27.3 g. of potassium phenylthiomethyldithiocarbamate keeping the reaction temperature below 30°C. by cooling. After another 2 hours, the mixture was poured into water and extracted with ethylene chloride. The ethylene chloride mixture was washed with water, dried, and saturated with dry hydrogen chloride. The resulting salt was collected by filtration and washed with acetone. The salt, on stirring with a mixture of 100 ml. of water and 300 ml. of chloroform, dissolved and removal and concentration of the chloroform layer gave 8.5 g. of the dithietane as a white solid, m.p. 50°-52°C.

후처리

  1. additionTo a mixture of 28.2 g
  2. extractionextracted with ethylene chloride
  3. washThe ethylene chloride mixture was washed with water
  4. customdried
  5. filtrationThe resulting salt was collected by filtration
  6. washwashed with acetone
  7. dissolutionof chloroform, dissolved
  8. customremoval and concentration of the chloroform layer
  9. customgave 8.5 g

출처 및 근거

ORD 기록
ord-aefb2e0d26a44920833aa411bb07852e
출처 데이터셋
uspto-grants-1976_08
특허 번호
US03975528

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