Triethylamine → HCID 18975625, 화합물

HRID 2393327노트

반응식

HRID 2393327 반응식
[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]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 879762,6-Xylyl isothiocyanateHCID 12227201HCID 12227201, 화합물

생성물 1

HCID 18975625HCID 18975625, 화합물수율 39.3%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-6625c77a72f04e8ea7be86a0aeae05ba
출처 데이터셋
uspto-grants-1998_09
특허 번호
US05807864

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