Sodium Bicarbonate → HCID 90017711, 화합물

HRID 1055004노트

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HRID 1055004 반응식
[CH2:1]([C:3]1[C:4]([NH:10][NH:11][C:12](=O)[CH2:13][CH2:14][C:15]2[N:19]([CH3:20])[N:18]=[C:17]([N:21]3[CH2:25][CH2:24][CH2:23][CH2:22]3)[N:16]=2)=[N:5][C:6]([CH3:9])=[N:7][CH:8]=1)[CH3:2].CC[N+](S(N=C(OC)[O-])(=O)=O)(CC)CC.C(=O)(O)[O-].[Na+]>O1CCCC1>[CH2:1]([C:3]1[C:4]2[N:5]([C:12]([CH2:13][CH2:14][C:15]3[N:19]([CH3:20])[N:18]=[C:17]([N:21]4[CH2:25][CH2:24][CH2:23][CH2:22]4)[N:16]=3)=[N:11][N:10]=2)[C:6]([CH3:9])=[N:7][CH:8]=1)[CH3:2]

참가 물질

5

반응물 3

HCID 516892Sodium BicarbonateHCID 2724994Methyl N-(triethylammoniosulfonyl)carbamateHCID 90017038HCID 90017038, 화합물

생성물 1

HCID 90017711HCID 90017711, 화합물수율 128.3%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
80 °C

실험 절차

N′-(5-Ethyl-2-methylpyrimidin-4-yl)-3-(1-methyl-3-(pyrrolidin-1-yl)-1H-1,2,4-triazol-5-yl)propanehydrazide (56.6 mg, 158 μmol) in tetrahydrofuran (4 ml) was added to Burgess reagent (155 mg, 632 μmol). The mixture was heated in a sealed tube at 80° C. for 1 h. Saturated sodium bicarbonate solution was added and extracted with dichloromethane. The organic layers were dried over sodium sulfate and concentrated to an oil to afford the desired product (69 mg) as a yellow solid which was used without further purification in the next step. MS: m/z=341.2 (M+H+)

후처리

  1. extractionextracted with dichloromethane
  2. dry with materialThe organic layers were dried over sodium sulfate
  3. concentrationconcentrated to an oil

출처 및 근거

ORD 기록
ord-922df7ab2a5d4cf6bd9ed24684fec3b8
출처 데이터셋
uspto-grants-2016_07
특허 번호
US09394311B2

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