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Trifluoroacetic acid → HCID 71554976, 화합물

HRID 2407535
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HRID 2407535 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([N:11]2[C:14]3([CH2:17][N:16]([C:18](OC(C)(C)C)=[O:19])[CH2:15]3)[CH2:13][CH2:12]2)(=[O:10])=[O:9])=[CH:4][CH:3]=1.FC(F)(F)C(O)=O.[Cl:32][C:33]1[CH:38]=[C:37]([Cl:39])[CH:36]=[CH:35][C:34]=1[CH2:40][N:41]=C=O.C(N(CC)CC)C>ClCCl.C(#N)C>[Cl:32][C:33]1[CH:38]=[C:37]([Cl:39])[CH:36]=[CH:35][C:34]=1[CH2:40][NH:41][C:18]([N:16]1[CH2:15][C:14]2([N:11]([S:8]([C:5]3[CH:4]=[CH:3][C:2]([F:1])=[CH:7][CH:6]=3)(=[O:9])=[O:10])[CH2:12][CH2:13]2)[CH2:17]1)=[O:19]
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참가 물질

7

반응물 4

HCID 6422Trifluoroacetic acid2회HCID 8471TriethylamineHCID 46127082,4-Dichlorobenzyl isocyanateHCID 86682348HCID 86682348, 화합물

생성물 1

HCID 71554976HCID 71554976, 화합물수율 91.1%

시약·촉매·용매 2

HCID 6342Acetonitrile
용매
HCID 6344Dichloromethane용매

실험 절차

To a solution of tert-butyl 1-(4-fluorophenylsulfonyl)-1,6-diazaspiro[3.3]heptane-6-carboxylate (452 mg, 1.27 mmol) in dichloromethane (8 mL) was added trifluoroacetic acid (489 μl, 6.34 mmol). After 2 h at ambient temperature, another amount of trifluoroacetic acid was added (300 μl, 3.89 mmol). The reaction mixture was stirred for 1.5 h at ambient temperature and concentrated under reduced pressure. The residue was partitioned in toluene (10 mL) and then concentrated, this procedure was repeated twice to give the unpurified amine (540 mg), which was used directly in the next step without further purification. To a solution of the obtained 1-(4-fluorophenylsulfonyl)-1,6-diazaspiro[3.3]heptanes in acetonitrile (10 mL) was added 2,4-dichloro-1-(isocyanatomethyl)benzene (216 μl, 1.47 mmol) followed by triethylamine (294 μl, 2.11 mmol) and the mixture was stirred for 1 h at ambient temperature. The solvent was evaporated in vacuo and the resulting solid was purified by chromatography (SiO2; heptane:ethyl acetate 1:4 to dichloromethane/methanol/ammonia 95:4.5:0.5) to give the titled compound (530 mg, 91%) as colorless solid. HRMS (EI): 457.0431 (exact mass calculated for C19H17Cl2FN3O3S ([M]+)=457.0430).

후처리

  1. concentrationconcentrated under reduced pressure
  2. customThe residue was partitioned in toluene (10 mL)
  3. concentrationconcentrated
  4. customto give the unpurified amine (540 mg), which
  5. customwas used directly in the next step without further purification
  6. stirringthe mixture was stirred for 1 h at ambient temperature
  7. customThe solvent was evaporated in vacuo
  8. customthe resulting solid was purified by chromatography (SiO2; heptane:ethyl acetate 1:4 to dichloromethane/methanol/ammonia 95:4.5:0.5)

출처 및 근거

ORD 기록
ord-dfb894586aee496a89eecd6b6de25e43
출처 데이터셋
uspto-grants-2014_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08809552B2

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