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Dibromomethane → 2-Furfurylimino-1,3-dithietane

HRID 1973575
ノート
印刷プレビュー

反応式

HRID 1973575 の反応式
[CH2:1]([NH:7][C:8](=[S:10])[S-:9])[C:2]1[O:6][CH:5]=[CH:4][CH:3]=1.[CH2:11]([NH+](CC)CC)C.C(Br)Br.C(N(CC)CC)C.S1CCS1>CN(C)C=O>[CH2:1]([N:7]=[C:8]1[S:9][CH2:11][S:10]1)[C:2]1[O:6][CH:5]=[CH:4][CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 3024DibromomethaneHCID 8471TriethylamineHCID 123092831,2-DithietaneHCID 21453310Triethylammonium furfuryldithiocarbamate

生成物 1

HCID 214532962-Furfurylimino-1,3-dithietane

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

このページの内容参加物実験手順後処理出典と根拠反応ノート

A mixture of 13.7 g. of triethylammonium furfuryldithiocarbamate, 10.5 ml. of methylene bromide, and 7.0 ml. of triethylamine in 100 ml. of dimethylformamide was stirred for several hours and then poured into ice-water. The oily product was partitioned into ether and the ether mixture was extracted with 3N hydrochloric acid. After extracting the acidic solution with methylene chloride, it was made basic with potassium hydroxide solution and re-extracted with methylene chloride. The methylene chloride mixture, after water washing, drying, and concentrating in vacuo afforded 4.9 g. of the desired dithietane as a yellow oil.

後処理

  1. additionA mixture of 13.7 g
  2. customThe oily product was partitioned into ether
  3. extractionthe ether mixture was extracted with 3N hydrochloric acid
  4. extractionAfter extracting the acidic solution with methylene chloride, it
  5. extractionre-extracted with methylene chloride
  6. dry with materialThe methylene chloride mixture, after water washing, drying
  7. concentrationconcentrating in vacuo
  8. customafforded 4.9 g

出典と根拠

ORDレコード
ord-cb184dfcc68f43e7838d7b7ada97fbf4
出典データセット
uspto-grants-1976_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US03997668

反応ノート

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