Carbon Disulfide → HCID 13021142、化合物

HRID 1278261ノート

反応式

HRID 1278261 の反応式
[CH2:1]([NH:4][CH2:5][CH2:6][CH3:7])[CH2:2][CH3:3].O1C[CH2:11][CH2:10][CH2:9]1.[C:13](=[S:15])=[S:14].C(Br)C=C>O>[CH2:9]([S:15][C:13](=[S:14])[N:4]([CH2:5][CH2:6][CH3:7])[CH2:1][CH2:2][CH3:3])[CH:10]=[CH2:11]

参加物

6

反応物 4

HCID 6348Carbon DisulfideHCID 7841Allyl bromideHCID 8028TetrahydrofuranHCID 8902Dipropylamine

生成物 1

HCID 13021142HCID 13021142、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

13.4 Grams of dipropylamine was added to 50 ml of tetrahydrofuran, and to this mixture being maintained a temperature at 0°-5° C., was added dropwise 5.0 gr of carbon disulfide over the period of 30 minutes under agitation. Thereafter, the mixture was maintained at a room temperature and 7.3 gr of allyl bromide was added dropwise thereto over the period of 30 minutes. The mixture was agitated at the same temperature for 3 hours to complete the reaction. The reaction mixture was poured into water and the separated organic substance was extracted twice with 30 ml of toluene and washed with diluted hydrochloric acid, followed by further washing with water. After removal of toluene by distillation to obtain 9.7 gr of the desired product.

後処理

  1. temperatureto this mixture being maintained a temperature at 0°-5° C.
  2. customover the period of 30 minutes
  3. customthe reaction
  4. extractionthe separated organic substance was extracted twice with 30 ml of toluene
  5. washwashed with diluted hydrochloric acid
  6. washby further washing with water
  7. customAfter removal of toluene
  8. distillationby distillation

出典と根拠

ORDレコード
ord-1fd0d85691b740f2b13e1ef6def5e7c2
出典データセット
uspto-grants-1981_07
特許番号
US04281016

反応ノート

読み込み中…