Ethyl difluoroacetate → HCID 178452595, 화합물

HRID 1509242노트

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HRID 1509242 반응식
[F:1][CH:2]([F:8])[C:3](OCC)=[O:4].O.[NH2:10][NH2:11].[C:12]1([C:18]2[C:28]([C:29]3[CH:34]=[CH:33][C:32]([C:35]4([NH:39][C:40](=[O:46])[O:41][C:42]([CH3:45])([CH3:44])[CH3:43])[CH2:38][CH2:37][CH2:36]4)=[CH:31][CH:30]=3)=[N:27][C:21]3[O:22][CH2:23][C:24](=S)[NH:25][C:20]=3[CH:19]=2)[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1>CN(C)C=O>[F:1][CH:2]([F:8])[C:3]([NH:10]/[N:11]=[C:24]1/[NH:25][C:20]2[CH:19]=[C:18]([C:12]3[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=3)[C:28]([C:29]3[CH:30]=[CH:31][C:32]([C:35]4([NH:39][C:40](=[O:46])[O:41][C:42]([CH3:45])([CH3:43])[CH3:44])[CH2:36][CH2:37][CH2:38]4)=[CH:33][CH:34]=3)=[N:27][C:21]=2[O:22][CH2:23]/1)=[O:4]

참가 물질

5

반응물 3

HCID 9961Ethyl difluoroacetateHCID 24654Hydrazine hydrate (1:1)HCID 86683631Tert-butyl (1-(4-(7-phenyl-2-thioxo-2,3-dihydro-1H-pyrido[2,3-b][1,4]oxazin-6-yl)phenyl)cyclobutyl)carbamate

생성물 1

HCID 178452595HCID 178452595, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
70 °C

실험 절차

Ethyl 2,2-difluoroacetate (0.43 ml, 4.10 mmol) and hydrazine monohydrate were heated to 60° C. in N,N-dimethylformamide (1 ml) for 30 minutes to give a colourless solution. Tert-butyl (1-(4-(7-phenyl-2-thioxo-2,3-dihydro-1H-pyrido[2,3-b][1,4]oxazin-6-yl)phenyl)cyclobutyl)carbamate (100 mg, 0.205 mmol) was added to the previous solution at room temperature. The resulting mixture was heated to 70° C. for 20 hours. The reaction mixture was concentrated under reduced pressure and the crude material (100 mg, quantitative yield) was used for the next step without further purification. LCMS (Method D): RT=1.37 min, M+1=564.

후처리

  1. customto give a colourless solution
  2. concentrationThe reaction mixture was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-839d9fed66214882a34d64879d27ede4
출처 데이터셋
uspto-grants-2015_12
특허 번호
US09221838B2

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