Triethylamine → HCID 13799783、化合物

HRID 1906380ノート

反応式

HRID 1906380 の反応式
C(N(CC)CC)C.Cl.[NH2:9][C:10]1([C:15]#[N:16])[CH2:14][CH2:13][CH2:12][CH2:11]1.[CH3:17][S:18](Cl)(=[O:20])=[O:19]>C(Cl)(Cl)Cl>[C:15]([C:10]1([NH:9][S:18]([CH3:17])(=[O:20])=[O:19])[CH2:14][CH2:13][CH2:12][CH2:11]1)#[N:16]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 202117581-Aminocyclopentane-1-carbonitrile--hydrogen chloride (1/1)2 回

生成物 1

HCID 13799783HCID 13799783、化合物収率 69.1%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒2 回

実験手順

To a stirred mixture of 20.2 g (0.2 mole) triethylamine and 200 ml chloroform cooled in an ice bath, 14.7 g (0.1 mole) 1-amino-1-cyanocyclopentane hydrochloride (the product of Example 14) were spooned in over ten minutes to give a red solution. To that mixture, 11.5 g (0.1 mole) methanesulfonyl chloride in 25 ml chloroform were added dropwise over 30 minutes. The reaction mixture was stirred 30 minutes. The reaction mixture was washed with 25 ml concentrated hydrochloric acid which had been diluted to 50 ml with ice water. The layers were phase separated. The organic layer was washed twice with 50 ml ice water, dried over magnesium sulfate and stripped to give 13 g of the above-identified amber oily product.

後処理

  1. temperaturecooled in an ice bath
  2. customwere spooned in over ten minutes
  3. customto give a red solution
  4. washThe reaction mixture was washed with 25 ml concentrated hydrochloric acid which
  5. additionhad been diluted to 50 ml with ice water
  6. customseparated
  7. washThe organic layer was washed twice with 50 ml ice water
  8. dry with materialdried over magnesium sulfate

出典と根拠

ORDレコード
ord-f0a2e6e13bb14d1c85eb93993bc4e3bf
出典データセット
uspto-grants-1987_03
特許番号
US04652556

反応ノート

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