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Hydrochloric Acid → HCID 46897236, 화합물

HRID 1966966
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HRID 1966966 반응식
C(N(CC)C(C)C)(C)C.CN(C(ON1N=NC2C=CC=CC1=2)=[N+](C)C)C.[B-](F)(F)(F)F.[O:32]=[C:33]1[N:37]([CH2:38][C:39]([OH:41])=O)[C:36](=[O:42])[C:35]2([CH2:47][CH2:46][CH2:45][CH2:44][CH2:43]2)[N:34]1[C:48]1[CH:53]=[CH:52][C:51]([CH3:54])=[CH:50][CH:49]=1.[C:55]1([CH:61]([NH2:65])[CH2:62][CH2:63][CH3:64])[CH:60]=[CH:59][CH:58]=[CH:57][CH:56]=1.Cl>CN1C(=O)CCC1>[O:32]=[C:33]1[N:37]([CH2:38][C:39]([NH:65][CH:61]([C:55]2[CH:60]=[CH:59][CH:58]=[CH:57][CH:56]=2)[CH2:62][CH2:63][CH3:64])=[O:41])[C:36](=[O:42])[C:35]2([CH2:47][CH2:46][CH2:45][CH2:44][CH2:43]2)[N:34]1[C:48]1[CH:53]=[CH:52][C:51]([CH3:54])=[CH:50][CH:49]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 5

HCID 313Hydrochloric AcidHCID 81531DiisopropylethylamineHCID 2733207O-(Benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium tetrafluoroborateHCID 36037851-Phenylbutan-1-amine2회HCID 66680556HCID 66680556, 화합물

생성물 1

HCID 46897236HCID 46897236, 화합물

시약·촉매·용매 1

HCID 13387N-methyl-2-pyrrolidone용매

실험 절차

170 μl (0.098 mmol, 0.1 eq.) of N,N-diisopropylethylamine and 204 mg (0.63 mmol, 2 eq.) of TBTU are added to a solution of 100 mg of (2,4-dioxo-1-p-tolyl-1,3-diazaspiro[4.5]dec-3-yl)acetic acid in 30 ml of NMP. The solution is stirred for 20 minutes, and 70 mg (0.47 mmol, 1.5 eq.) of 1-phenylbutylamine (starting material 3) are added. The reaction medium is stirred overnight at room temperature. It is then poured into 1N hydrochloric acid solution and extracted with ethyl acetate. The organic phase is then washed with water, then with 1N sodium hydroxide solution, and then again with water. It is dried over sodium sulfate. The residue is precipitated from dichloromethane and heptane. 2-(2,4-Dioxo-1-p-tolyl-1,3-diazaspiro[4.5]dec-3-yl)-N-(1-phenylbutyl)acetamide is obtained in the form of a white solid.

후처리

  1. stirringThe reaction medium is stirred overnight at room temperature
  2. extractionextracted with ethyl acetate
  3. washThe organic phase is then washed with water
  4. dry with materialIt is dried over sodium sulfate
  5. customThe residue is precipitated from dichloromethane and heptane

출처 및 근거

ORD 기록
ord-5e277f2a924d49a2b2c3c94c58edaf87
출처 데이터셋
uspto-grants-2013_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08420681B2

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