Hydrochloric Acid → HCID 178448596, 화합물

HRID 2206443노트

반응식

HRID 2206443 반응식
[CH2:1]([NH2:5])[CH2:2][CH2:3][CH3:4].C=O.Cl.[CH2:9](O)C.[N:12]1[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=1[C:18]([C:20]1[CH:25]=[CH:24][C:23]([CH3:26])=[CH:22][CH:21]=1)=O.[C:27]1([B-:33]([C:46]2[CH:51]=[CH:50][CH:49]=[CH:48][CH:47]=2)([C:40]2[CH:45]=[CH:44][CH:43]=[CH:42][CH:41]=2)[C:34]2[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=2)[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=1.[Na+]>C(#N)C.CO>[C:46]1([B-:33]([C:27]2[CH:28]=[CH:29][CH:30]=[CH:31][CH:32]=2)([C:34]2[CH:35]=[CH:36][CH:37]=[CH:38][CH:39]=2)[C:40]2[CH:45]=[CH:44][CH:43]=[CH:42][CH:41]=2)[CH:47]=[CH:48][CH:49]=[CH:50][CH:51]=1.[CH2:1]([N:5]1[C:18]([C:20]2[CH:25]=[CH:24][C:23]([CH3:26])=[CH:22][CH:21]=2)=[C:13]2[CH:14]=[CH:15][CH:16]=[CH:17][N+:12]2=[CH:9]1)[CH2:2][CH2:3][CH3:4]

참가 물질

9

반응물 6

HCID 313Hydrochloric AcidHCID 702EthanolHCID 712FormaldehydeHCID 8007ButylamineHCID 2723787Sodium TetraphenylborateHCID 3018781(4-Methylphenyl)(pyridin-2-yl)methanone

생성물 1

HCID 178448596HCID 178448596, 화합물수율 72%

시약·촉매·용매 2

HCID 887Methanol용매2회HCID 6342Acetonitrile용매

실험 절차

was prepared according to general procedure (A), in which 25 μl n-butylamine (0.25 mmol, 1 equiv), 28 μl formalin (0.37 mmol, 1.5 equiv), 82 μl 3.05 M hydrochloric acid in ethanol (0.25 mmol, 1 equiv) and 49 mg pyridin-2-yl(p-tolyl)methanone (0.25 mmol, 1 equiv) were combined in 0.50 mL acetonitrile and maintained at room temperature for 12 hours. The crude material was then dissolved in 1.0 mL methanol and then 94 mg sodium tetraphenylborate (0.27 mmol, 1.1 equiv) in 1.0 mL methanol was added drop wise while stirring vigorously. The heterogeneous mixture was stirred vigorously for 3 hours at room temperature until the solid became a fine suspension, which was then filtered, washed with 500 μl of methanol and dried under high vacuum at 0.2 Torr to obtain 105 mg 2-butyl-1-(p-tolyl)-2H-imidazo[1,5-a]pyridin-4-ium tetraphenylborate (0.18 mmol, a 72% yield) as a white solid.

후처리

  1. customwas prepared
  2. stirringThe heterogeneous mixture was stirred vigorously for 3 hours at room temperature until the solid
  3. filtrationwas then filtered
  4. washwashed with 500 μl of methanol
  5. customdried under high vacuum at 0.2 Torr

출처 및 근거

ORD 기록
ord-be05a3522839429a8713492dac078490
출처 데이터셋
uspto-grants-2016_06
특허 번호
US09371448B2

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