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Triethylamine → HCID 58551215, 화합물

HRID 2204258
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HRID 2204258 반응식
[CH2:1]([C:3]1[CH:30]=[CH:29][C:6]([C:7]([N:9]2[CH2:14][CH2:13][C:12]3([O:19][C:18]4[CH:20]=[C:21]([CH:24]=O)[CH:22]=[CH:23][C:17]=4[N:16]4[CH:26]=[CH:27][CH:28]=[C:15]34)[CH2:11][CH2:10]2)=[O:8])=[CH:5][C:4]=1[O:31][CH3:32])[CH3:2].C[CH2:34][N:35](CC)[CH2:36]C>CN(C=O)C>[CH3:34][N:35]([CH2:24][C:21]1[CH:22]=[CH:23][C:17]2[N:16]3[CH:26]=[CH:27][CH:28]=[C:15]3[C:12]3([CH2:13][CH2:14][N:9]([C:7]([C:6]4[CH:29]=[CH:30][C:3]([CH2:1][CH3:2])=[C:4]([O:31][CH3:32])[CH:5]=4)=[O:8])[CH2:10][CH2:11]3)[O:19][C:18]=2[CH:20]=1)[CH3:36]
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참가 물질

4

반응물 2

HCID 8471TriethylamineHCID 58551190HCID 58551190, 화합물

생성물 1

HCID 58551215HCID 58551215, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A solution of 1′-(4-ethyl-3-methoxybenzoyl)spiro[benzo[b]pyrrolo[1,2-d][1,4]oxazine-4,4′-piperidine]-7-carbaldehyde (88 mg, 0.20 mmol) N,N-dimethylamine hydrochloride (83 mg, 1.0 mmol), Et3N (140 μL, 1.0 mmol) and NaHB(OAc)3 (130 mg, 0.60 mmol) in DMF (1 mL) was stirred at room temperature overnight. The reaction mixture was filtered and purified by reverse phase LC-MS (10-99% CH3CN/H2O) to yield (7-((dimethylamino)methyl)spiro[benzo[b]pyrrolo[1,2-d][1,4]oxazine-4,4′-piperidine]-1′-yl)(4-ethyl-3-methoxyphenyl)methanone. ESI-MS m/z calc. 459.6, found 460.5 (M+1)+; Retention time: 1.40 minutes (3 min run).

후처리

  1. filtrationThe reaction mixture was filtered
  2. custompurified by reverse phase LC-MS (10-99% CH3CN/H2O)

출처 및 근거

ORD 기록
ord-b2b0c2e5f3f04e50a5bd1bbd510ee72d
출처 데이터셋
uspto-grants-2016_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09365588B2

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