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Dimethylformamide → HCID 11668908, 화합물

HRID 2244977
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HRID 2244977 반응식
[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1NCC(O)=O.[Cl:13][C:14]1[CH:19]=[CH:18][C:17]([N:20]=[C:21]=[O:22])=[CH:16][CH:15]=1.Cl.C([N:31]1[CH2:36][CH2:35][CH2:34][CH2:33][CH:32]1CN)(OC(C)(C)C)=O.F[P-](F)(F)(F)(F)F.[N:46]1(O[P+](N(C)C)(N(C)C)N(C)C)[C:50]2C=CC=CC=2N=N1.[CH3:66][N:67]([CH:69]=[O:70])C>O.CCOC(C)=O>[NH:31]1[CH2:32][CH2:33][CH:34]([CH2:66][NH:67][C:69](=[O:70])[CH:50]([C:3]2[CH:4]=[CH:5][CH:6]=[CH:7][C:2]=2[F:1])[NH:46][C:21]([NH:20][C:17]2[CH:18]=[CH:19][C:14]([Cl:13])=[CH:15][CH:16]=2)=[O:22])[CH2:35][CH2:36]1
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참가 물질

8

반응물 5

HCID 6228Dimethylformamide2회HCID 76934-Chlorophenyl IsocyanateHCID 151348Benzotriazol-1-yloxy-tris(dimethylamino)phosphonium hexafluorophosphateHCID 5171030N-o-FluorophenylglycineHCID 45072188tert-Butyl 2-(aminomethyl)piperidine-1-carboxylate--hydrogen chloride (1/1)

생성물 1

HCID 11668908
HCID 11668908, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 8857Ethyl Acetate용매

실험 절차

To a solution of 2-fluorophenylglycine (59 mg, 0.35 mmol) in DMF (4 mL), 4-chlorophenylisocyanate (54 mg, 0.35 mmol) was added. The mixture was stirred at room temperature overnight. To the solution, a solution of N-BOC-aminomethylpiperidine hydrochloride (105 mg, 0.42 mmol) and TEA (0.150 mL, 1.08 mmol) in DMF (4 mL) was added, followed by addition of BOP (239 mg, 0.54 mmol). The mixture was then stirred at room temperature overnight. EtOAc and H2O were added. The organic layer was separated, dried over Na2SO4, concentrated in vacuo.

후처리

  1. stirringThe mixture was then stirred at room temperature overnight
  2. customThe organic layer was separated
  3. dry with materialdried over Na2SO4
  4. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-fef33255059a4f9590e7a6568b4ed735
출처 데이터셋
uspto-grants-2010_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07678913B2

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