Triethylamine → HCID 18975625、化合物

HRID 2393327ノート

反応式

HRID 2393327 の反応式
[CH2:1]([NH:3][CH2:4][CH2:5][C:6]([OH:8])=[O:7])[CH3:2].[CH3:9][C:10]1[CH:15]=[CH:14][CH:13]=[C:12]([CH3:16])[C:11]=1[N:17]=[C:18]=[S:19].C(N(CC)CC)C>C(Cl)Cl>[CH3:16][C:12]1[CH:13]=[CH:14][CH:15]=[C:10]([CH3:9])[C:11]=1[NH:17][C:18](=[S:19])[N:3]([CH2:4][CH2:5][C:6]([OH:8])=[O:7])[CH2:1][CH3:2]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 879762,6-Xylyl isothiocyanateHCID 12227201HCID 12227201、化合物

生成物 1

HCID 18975625HCID 18975625、化合物収率 39.3%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A mixture of 3-ethylaminopropionic acid (19.8 g), 2,6-dimethylphenyl-isothiocyanate (16.3 g), triethylamine (20 g) and methylene chloride (200 mL) was heated at reflux for 3 hours. The cooled reaction mixture was extracted with 1N NaOH (150 mL). The aqueous layer was separated and acidified with 2N HCl. The solid formed was collected by filtration. Recrystallization from ethanol afforded the title compound (11 g) as a white solid, m.p. 115°-118° C.

後処理

  1. temperaturewas heated
  2. temperatureat reflux for 3 hours
  3. customThe cooled reaction mixture
  4. extractionwas extracted with 1N NaOH (150 mL)
  5. customThe aqueous layer was separated
  6. customThe solid formed
  7. filtrationwas collected by filtration
  8. customRecrystallization from ethanol

出典と根拠

ORDレコード
ord-6625c77a72f04e8ea7be86a0aeae05ba
出典データセット
uspto-grants-1998_09
特許番号
US05807864

反応ノート

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