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

HRID 1973580ノート

反応式

HRID 1973580 の反応式
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

参加物

7

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

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 two 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.

後処理

  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

出典と根拠

ORDレコード
ord-db8ffea6e4bc4bf69032e10b311aa933
出典データセット
uspto-grants-1976_12
特許番号
US03997668

反応ノート

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