Triethylamine → HCID 71612644, 화합물

HRID 516811노트

반응식

HRID 516811 반응식
Cl.[NH2:2][CH2:3][CH:4]([OH:13])[CH2:5][O:6][C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1.Cl[CH2:15][C:16]([N:18]1[CH2:22][CH2:21][CH2:20][CH:19]1[C:23]#[N:24])=[O:17].C(N(CC)CC)C>ClCCl>[OH:13][CH:4]([CH2:5][O:6][C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1)[CH2:3][NH:2][CH2:15][C:16]([N:18]1[CH2:22][CH2:21][CH2:20][CH:19]1[C:23]#[N:24])=[O:17]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 27250721-Amino-3-phenoxypropan-2-ol hydrochlorideHCID 154801851-(2-Chloroacetyl)pyrrolidine-2-carbonitrile

생성물 1

HCID 71612644HCID 71612644, 화합물수율 33.6%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A solution of 1-amino-3-phenoxypropan-2-ol hydrochloride (7.9 g, 38.8 mmol) and 1-(2-chloroacetyl)pyrrolidine-2-carbonitrile (6.1 g, 35.3 mmol) in DCM (250 mL) was added triethylamine (15 mL, 106 mmol). The mixture was stirred at room temperature overnight. After the TLC showed that the reaction was complete, the mixture was washed by brine. The aqueous solution was extracted with dichloromethane (DCM) (3×100 mL) and the combined DCM solution was concentrated to give a crude product, which was purified by column chromatography to give 3.5 g of 1-(2-(2-hydroxy-3-phenoxypropylamino)acetyl)pyrrolidine-2-carbonitrile (as shown at 6). Yield was 33.6%.

후처리

  1. washthe mixture was washed by brine
  2. extractionThe aqueous solution was extracted with dichloromethane (DCM) (3×100 mL)
  3. concentrationthe combined DCM solution was concentrated
  4. customto give a crude product, which
  5. customwas purified by column chromatography

출처 및 근거

ORD 기록
ord-79e546d14e7e495aa4b9737f448d38e1
출처 데이터셋
uspto-grants-2015_08
특허 번호
US09115082B2

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