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Potassium Carbonate → (S)-2-(4-amino-3-chloro-5-trifluoromethyl-benzyl)-1-(4-dimethylamino-piperidin-1-yl)-4-[4-(2-oxo-1,2,4,5-tetrahydro-1,3-benzodiazepin-3-yl)-piperidin-1-yl]-butan-1,4-dione

HRID 736942
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인쇄 미리보기

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HRID 736942 반응식
CN(C(ON1N=NC2C=CC=CC1=2)=[N+](C)C)C.[B-](F)(F)(F)F.C(N(C(C)C)C(C)C)C.[CH3:32][N:33]([CH3:40])[CH:34]1[CH2:39][CH2:38][NH:37][CH2:36][CH2:35]1.[NH2:41][C:42]1[C:73]([C:74]([F:77])([F:76])[F:75])=[CH:72][C:45]([CH2:46][C@@H:47]([CH2:51][C:52](=[O:71])[N:53]2[CH2:58][CH2:57][CH:56]([N:59]3[CH2:65][CH2:64][C:63]4[CH:66]=[CH:67][CH:68]=[CH:69][C:62]=4[NH:61][C:60]3=[O:70])[CH2:55][CH2:54]2)[C:48](O)=[O:49])=[CH:44][C:43]=1[Cl:78].C([O-])([O-])=O.[K+].[K+]>CN(C=O)C>[NH2:41][C:42]1[C:73]([C:74]([F:76])([F:75])[F:77])=[CH:72][C:45]([CH2:46][C@@H:47]([CH2:51][C:52]([N:53]2[CH2:58][CH2:57][CH:56]([N:59]3[CH2:65][CH2:64][C:63]4[CH:66]=[CH:67][CH:68]=[CH:69][C:62]=4[NH:61][C:60]3=[O:70])[CH2:55][CH2:54]2)=[O:71])[C:48]([N:37]2[CH2:38][CH2:39][CH:34]([N:33]([CH3:40])[CH3:32])[CH2:35][CH2:36]2)=[O:49])=[CH:44][C:43]=1[Cl:78]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 5

HCID 11430Potassium CarbonateHCID 81531DiisopropylethylamineHCID 417391N,N-Dimethylpiperidin-4-amineHCID 2733207O-(Benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium tetrafluoroborateHCID 68591515(S)-2-(4-amino-3-chloro-5-trifluoromethyl-benzyl)-4-oxo-4-[4-(2-oxo-1,2,4,5-tetrahydro-1,3-benzodiazepin-3-yl)-piperidin-1-yl]-butanoic acid

생성물 1

HCID 57848212
(S)-2-(4-amino-3-chloro-5-trifluoromethyl-benzyl)-1-(4-dimethylamino-piperidin-1-yl)-4-[4-(2-oxo-1,2,4,5-tetrahydro-1,3-benzodiazepin-3-yl)-piperidin-1-yl]-butan-1,4-dione

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

80.3 mg (0.25 mmol) TBTU, 0.21 mL (1.2 mmol) ethyldiisopropylamine and 38.5 mg (0.3 mmol) dimethyl-piperidin-4-yl-amine were added to a solution of 130 mg (0.24 mmol) (S)-2-(4-amino-3-chloro-5-trifluoromethyl-benzyl)-4-oxo-4-[4-(2-oxo-1,2,4,5-tetrahydro-1,3-benzodiazepin-3-yl)-piperidin-1-yl]-butanoic acid in 10 mL DMF and the reaction mixture was stirred overnight at RT. The reaction solution was poured into 80 mL 15% K2CO3 solution, stirred for 10 min at RT, the precipitated substance was suction filtered, washed with 5 mL water and dried in the air over the weekend. Then the product was purified by chromatography using HPLC.

후처리

  1. stirringstirred for 10 min at RT
  2. filtrationfiltered
  3. washwashed with 5 mL water
  4. customdried in the air over the weekend
  5. customThen the product was purified by chromatography

출처 및 근거

ORD 기록
ord-4ed3dbde9fc544ffa4d97abd5cb99b99
출처 데이터셋
uspto-grants-2009_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07595312B2

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