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Phosgene → HCID 70650772, 화합물

HRID 1425651
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HRID 1425651 반응식
[O:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[CH2:6][O:7][CH2:8][C:9]1[CH:10]=[C:11]([CH:14]=[CH:15][CH:16]=1)[CH2:12][NH2:13].[C:17](Cl)(Cl)=[O:18].[S:21]1[C:25]2=[N:26][CH:27]=[CH:28][CH:29]=[C:24]2[C:23]([OH:30])=[N:22]1>C1(C)C=CC=CC=1>[O:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[CH2:6][O:7][CH2:8][C:9]1[CH:10]=[C:11]([CH:14]=[CH:15][CH:16]=1)[CH2:12][NH:13][C:23]([N:22]1[C:17](=[O:18])[C:24]2[C:25](=[N:26][CH:27]=[CH:28][CH:29]=2)[S:21]1)=[O:30]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6371PhosgeneHCID 16784344(3-{[(furan-2-yl)methoxy]methyl}phenyl)methanamineHCID 178519011HCID 178519011, 화합물

생성물 1

HCID 70650772HCID 70650772, 화합물

시약·촉매·용매 1

HCID 1140Toluene용매

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온도
60 °C

실험 절차

A solution of 3-(furan-2-ylmethoxymethyl)benzylamine (218 mg, 1 mmol) in toluene (10 ml) is admixed at 25° C. with phosgene (5 ml, 10 mmol; 20% solution in toluene) and heated to reflux. After 3 h, the mixture is filtered and the filtrate is concentrated. The residue is taken up in THF (25 ml) and admixed with compound 1 (122 mg, 0.8 mmol). The mixture is stirred at 60° C. for 3 h. The reaction is monitored by HPLC-MS. The solvent is reduced, and the product crystallizes. C20H17N3O4S, Mw 395.44. Yield: 239 mg (75.7%).

후처리

  1. temperatureheated to reflux
  2. filtrationthe mixture is filtered
  3. concentrationthe filtrate is concentrated
  4. customthe product crystallizes

출처 및 근거

ORD 기록
ord-33b402a821bf4ff78fececfb49c0014c
출처 데이터셋
uspto-grants-2015_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08933024B2

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