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1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide → N-BOC-4-aminobenzoyl methionine methyl ester

HRID 356076
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HRID 356076 반응식
[C:1](NC1C=CC(C(O)=O)=CC=1)([O:3][C:4]([CH3:7])([CH3:6])[CH3:5])=[O:2].Cl.[CH3:19][O:20][C:21](=[O:28])[C@H:22]([CH2:24][CH2:25][S:26][CH3:27])[NH2:23].CCN=C=N[CH2:34][CH2:35][CH2:36][N:37](C)C.[OH:40][C:41]1C2N=NNC=2[CH:44]=[CH:43][CH:42]=1>C(Cl)Cl.C(N(CC)CC)C>[CH3:19][O:20][C:21](=[O:28])[C@H:22]([CH2:24][CH2:25][S:26][CH3:27])[N:23]([C:41](=[O:40])[C:42]1[CH:34]=[CH:35][C:36]([NH2:37])=[CH:44][CH:43]=1)[C:1]([O:3][C:4]([CH3:5])([CH3:6])[CH3:7])=[O:2]
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참가 물질

7

반응물 4

HCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 27559314-{[(Tert-butoxy)carbonyl]amino}benzoic acidHCID 11435579L-Methionine, methyl ester, hydrochlorideHCID 178418300HCID 178418300, 화합물

생성물 1

HCID 67564255N-BOC-4-aminobenzoyl methionine methyl ester수율 71.3%

시약·촉매·용매 2

HCID 6344
Dichloromethane
용매
2회
HCID 8471Triethylamine용매

실험 절차

Into a dried, nitrogen filled flask was placed N-BOC-4-aminobenzoic acid (8.77 g, 36.97 mmol) in dry CH2Cl2 (148 ml) along with methionine methyl ester hydrochloride (8.12 g, 40.66 mmol). This solution was cooled in an ice bath and triethylamine (6.7 ml), EDCI (7.80 g, 40.66 mmol) and hydroxybenzotriazole (HOBT, 5.50 g, 40.66 mmol) were added. The mixture was stirred overnight, diluted with more CH2Cl2 and was extracted 3 times each with 1M HCl, 1M NaHCO3 and water. The CH2Cl2 was dried over MgSO4 and the solvent was removed in vacuo. The solid was recrystallized from ethyl acetate/ hexanes to yield 9.72 g (71.3%) of pure product. mp 184°-185° C.; 1H NMR (CDCl3) 1.53 (9 H, s), 2.06-2.18 (4 H, m), 2.23-2.33 (1 H, m), 2.59 (2 H, t, J=7.6 Hz), 3.80 (3 H, s), 4.92 (1 H, m), 7.45 (2 H, d, J=8.7 Hz), 7.77 (2 H, d, J=8.7 Hz); 13C NMR (CDCl3) 15.59, 28.34, 30.15, 31.64, 52.10, 52.73, 81.20, 117.73, 127.8, 128.33, 141.88, 152.33, 166.50, 172.75; anal. calc. for C18H26N2O5S, C: 56.53, H: 6.85, N: 7.29; found, C: 56.47, H: 6.86, N: 7.29; m/ z (EI) 382 (M).

후처리

  1. temperatureThis solution was cooled in an ice bath
  2. extractionwas extracted 3 times each with 1M HCl, 1M NaHCO3 and water
  3. dry with materialThe CH2Cl2 was dried over MgSO4
  4. customthe solvent was removed in vacuo
  5. customThe solid was recrystallized from ethyl acetate/ hexanes

출처 및 근거

ORD 기록
ord-60dd2c7aacd54c3396cf200f3ec45eeb
출처 데이터셋
uspto-grants-1998_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05834434

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