Triethylamine → HCID 15034359, 화합물

HRID 359064노트

반응식

HRID 359064 반응식
[C:1]1([O:7][CH2:8][CH:9]2[O:11][CH2:10]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.Cl.[CH2:13]([NH:20][CH2:21][CH2:22][C:23]1[CH:28]=[CH:27][C:26]([OH:29])=[CH:25][CH:24]=1)[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1.C(N(CC)CC)C>C(O)(C)C>[CH2:13]([N:20]([CH2:21][CH2:22][C:23]1[CH:24]=[CH:25][C:26]([OH:29])=[CH:27][CH:28]=1)[CH2:10][CH:9]([OH:11])[CH2:8][O:7][C:1]1[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1)[C:14]1[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 31217Phenyl glycidyl etherHCID 3042571Phenol, 4-(2-((phenylmethyl)amino)ethyl)-, hydrochloride

생성물 1

HCID 15034359HCID 15034359, 화합물수율 88.7%

시약·촉매·용매 1

HCID 3776Isopropanol용매

실험 절차

A mixture of phenylglycidyl ether (8.0 g), N-benzyltyramine hydrochloride (13.0 g) and triethylamine (7.5 ml) in isopropanol (200 ml) was heated to reflux for 3hours. The solvent was evaporated and toluene was added to the residue. Volatile material was evaporated. The residue was purified by chromatography on K60 silica (300 g) using a gradient mixture of methanol in dichloromethane (1 to 2% methanol). Thus was obtained 4-[2-(N-benzyl-N-(2-hydroxy-3-phenoxypropyl)amino)ethyl]phenol (16.5 g) as an oil which slowly crystallised, m.p. 103°-5° C.: NMR: 2.55-2.85[m,6H, CHCH2NHCH2CH2 ]; 3.65-4.05 [m,5H, PhOCH2CHOH +PhCH2 ]; 6.65-7.4[m,14H, aromatic H].

후처리

  1. temperaturewas heated
  2. temperatureto reflux for 3hours
  3. customThe solvent was evaporated
  4. additiontoluene was added to the residue
  5. customVolatile material was evaporated
  6. customThe residue was purified by chromatography on K60 silica (300 g)
  7. additiona gradient mixture of methanol in dichloromethane (1 to 2% methanol)

출처 및 근거

ORD 기록
ord-b8cc23800e474d20a7d87ffc089cbf50
출처 데이터셋
uspto-grants-1991_03
특허 번호
US04999377

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