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Triethylamine → HCID 68722905, 화합물

HRID 2381030
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HRID 2381030 반응식
[CH3:1][O:2][C:3](=[O:32])[C@@H:4]([NH:21][C:22]([O:24][CH2:25][C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1)=[O:23])[CH2:5][C:6]1[CH:11]=[CH:10][C:9]([O:12][CH2:13][C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)=[C:8]([OH:20])[CH:7]=1.[N:33]1([C:38](Cl)=[O:39])[CH2:37][CH2:36][CH2:35][CH2:34]1.C(N(CC)CC)C>ClCCl.CN(C1C=CN=CC=1)C>[CH2:13]([O:12][C:9]1[CH:10]=[CH:11][C:6]([CH2:5][C@H:4]([NH:21][C:22]([O:24][CH2:25][C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=2)=[O:23])[C:3]([O:2][CH3:1])=[O:32])=[CH:7][C:8]=1[O:20][C:38]([N:33]1[CH2:37][CH2:36][CH2:35][CH2:34]1)=[O:39])[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1
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참가 물질

6

반응물 3

HCID 8471Triethylamine2회HCID 709371-Pyrrolidinecarbonyl chloride2회HCID 11316490(S)-2-Benzyloxycarbonylamino-3-(4-benzyloxy-3-hydroxy-phenyl)-propionic acid methyl ester

생성물 1

HCID 68722905HCID 68722905, 화합물

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매
HCID 6344
Dichloromethane
용매
3회

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온도
40 °C

실험 절차

(S)-2-Benzyloxycarbonylamino-3-(4-benzyloxy-3-hydroxy-phenyl)-propionic acid methyl ester (434 mg) was dissolved in dichloromethane (7 ml) and a solution of 1-pyrrolidinylcarbonyl chloride (200 mg) in dichloromethane (2 ml) was added. Triethylamine (0.22 ml) was added dropwise followed by a catalytic amount of DMAP. The mixture was stirred and heated at 40° C. overnight. The reaction was monitored by HPLC/MS and further portions of 1-pyrrolidinylcarbonyl chloride (400 mg) and triethylamine (0.4 ml) were added and heating continued at 55 C for 48 hours. The reaction mixture was diluted with dichloromethane and washed with dil HCl, with aq sodium bicarbonate and with brine. Drying (MgSO4) and evaporation gave the crude product. Silca gel chromatography, eluting with mixtures of ethyl acetate-hexane gave pyrrolidine-1-carboxylic acid 2-benzyloxy-5-((S)-2-benzyloxycarbonylamino-2-methoxycarbonyl-ethyl)-phenyl ester as a colourless gum, 364 mg; Rf 0.3 (ethyl acetate-hexane 1:1); HPLC/MS retention time 7.31 min, m/z 533 (MH+).

후처리

  1. additionwere added
  2. temperatureheating
  3. washwashed with dil HCl, with aq sodium bicarbonate and with brine
  4. customDrying
  5. custom(MgSO4) and evaporation
  6. customgave the crude product
  7. washSilca gel chromatography, eluting with mixtures of ethyl acetate-hexane

출처 및 근거

ORD 기록
ord-ff6dba950d1a403a9f954be8d0d33449
출처 데이터셋
uspto-grants-2012_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08258097B2

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