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Triethylamine → 3-(2-Iodo-phenylcarbamoyl)-azetidine-1-carboxylic acid benzyl ester

HRID 528746
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HRID 528746 반응식
[I:1]NC1C=CC=CC=1.F[P-](F)(F)(F)(F)F.[N:16]1(O[P+](N(C)C)(N(C)C)N(C)C)[C:20]2[CH:21]=[CH:22][CH:23]=[CH:24][C:19]=2N=N1.[CH2:36]([O:43][C:44]([N:46]1[CH2:49][CH:48]([C:50]([OH:52])=O)[CH2:47]1)=[O:45])[C:37]1[CH:42]=[CH:41][CH:40]=[CH:39][CH:38]=1.C(N(CC)CC)C.C([O-])([O-])=O.[Na+].[Na+]>C(#N)C>[CH2:36]([O:43][C:44]([N:46]1[CH2:49][CH:48]([C:50](=[O:52])[NH:16][C:20]2[CH:21]=[CH:22][CH:23]=[CH:24][C:19]=2[I:1])[CH2:47]1)=[O:45])[C:37]1[CH:42]=[CH:41][CH:40]=[CH:39][CH:38]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 5

HCID 8471Triethylamine2회HCID 10340Sodium CarbonateHCID 151348Benzotriazol-1-yloxy-tris(dimethylamino)phosphonium hexafluorophosphate2회HCID 109882141-[(Benzyloxy)carbonyl]azetidine-3-carboxylic acidHCID 18447960Iodoaniline

생성물 1

HCID 67456254
3-(2-Iodo-phenylcarbamoyl)-azetidine-1-carboxylic acid benzyl ester

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

To 1.0 g (4.57 mmol) iodoaniline in 30 mL acetonitrile were added 2.22 g (5.02 mmol) BOP, 1.78 g (4.57 mmol) azetidine-1,3-dicarboxylic acid monobenzyl ester (route 13, step a), 0.6 mL (4.57 mmol) triethylamine, and the mixture was stirred at room temperature for 16 hours. 0.6 mL (4.57 mmol) triethylamine was added and the mixture was stirred for 2 hours. 2.22 g (5.02 mmol) BOP was added and the mixture was stirred at room temperature for 16 hours. 30 mL 1 M aqueous Na2CO3 was added and the mixture was extracted with EtOAc (2×30 mL), the organic layers were combined, washed with 30 mL brine then dried with Na2SO4. After filtration and evaporation of the solvent the product was purified by column chromatography (silica, heptane/EtOAc 7:3).

후처리

  1. stirringthe mixture was stirred for 2 hours
  2. stirringthe mixture was stirred at room temperature for 16 hours
  3. extractionthe mixture was extracted with EtOAc (2×30 mL)
  4. washwashed with 30 mL brine
  5. dry with materialthen dried with Na2SO4
  6. filtrationAfter filtration and evaporation of the solvent the product
  7. customwas purified by column chromatography (silica, heptane/EtOAc 7:3)

출처 및 근거

ORD 기록
ord-4d605f15ccd44d6ab539dec074437487
출처 데이터셋
uspto-grants-2016_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09346816B2

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