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Triethylamine → HCID 58551319, 화합물

HRID 2204065
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HRID 2204065 반응식
[NH4+].[Cl-].CC[N:5](CC)CC.[C:10]([O:14][C:15]([N:17]1[CH2:37][CH2:36][C:20]2([C:25]3=[CH:26][CH:27]=[CH:28][N:24]3[C:23]3[CH:29]=[CH:30][C:31]([C:33]([OH:35])=O)=[CH:32][C:22]=3[O:21]2)[CH2:19][CH2:18]1)=[O:16])([CH3:13])([CH3:12])[CH3:11].CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F>CN(C=O)C.C(OCC)(=O)C>[C:33]([C:31]1[CH:30]=[CH:29][C:23]2[N:24]3[CH:28]=[CH:27][CH:26]=[C:25]3[C:20]3([CH2:19][CH2:18][N:17]([C:15]([O:14][C:10]([CH3:13])([CH3:12])[CH3:11])=[O:16])[CH2:37][CH2:36]3)[O:21][C:22]=2[CH:32]=1)(=[O:35])[NH2:5]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 8471Triethylamine2회HCID 25517Ammonium ChlorideHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 58550886HCID 58550886, 화합물

생성물 1

HCID 58551319HCID 58551319, 화합물수율 89%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매2회
HCID 8857Ethyl Acetate용매

실험 절차

A solution of NH4Cl (1.4 mL, 40 mmol) and Et3N (5.6 mL, 40 mmol) in DMF (6 mL) was added to a solution of 1-tert-butoxycarbonylspiro[piperidine-4,4′-pyrrolo[2,1-c][1,4]benzoxazine]-7′-carboxylic acid (3.1 g, 8.0 mmol), HATU (3.3 g, 8.8 mmol), and Et3N (2.5 mL, 18 mmol) in DMF (6 mL). The mixture was stirred at room temperature for 1 h. The reaction mixture was diluted with ethyl acetate and was washed with saturated sodium bicarbonate solution. The organics were dried over sodium sulfate, filtered and evaporated. Purification of the residue by silica gel chromatography eluting with 0-100% EtOAc in Hexanes gave tert-butyl 7′-carbamoylspiro[piperidine-4,4′-pyrrolo[2,1-c][1,4]benzoxazine]-1-carboxylate (2.7 g, 89%). ESI-MS m/z calc. 383.4, found 384.7 (M+1)+. Retention time: 1.60 minutes (3 min run).

후처리

  1. washwas washed with saturated sodium bicarbonate solution
  2. dry with materialThe organics were dried over sodium sulfate
  3. filtrationfiltered
  4. customevaporated
  5. customPurification of the residue by silica gel chromatography
  6. washeluting with 0-100% EtOAc in Hexanes

출처 및 근거

ORD 기록
ord-097daedcdf8840e2a4911556f4311e8a
출처 데이터셋
uspto-grants-2016_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09365588B2

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