Diisopropylethylamine → 5-chloro-thiophene-2-carboxylic acid-N-{1-[3-methyl-4-(4-ethyl-piperazin-1-yl-carbonyl)-phenylcarbamoyl]-ethyl}-amide

HRID 15109

반응식

HRID 15109 반응식
[Cl:1][C:2]1[S:6][C:5]([C:7]([NH:9][CH:10]([CH3:14])[C:11]([OH:13])=O)=[O:8])=[CH:4][CH:3]=1.[CH3:15]CN(C(C)C)C(C)C.CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.[CH2:48]([N:50]1[CH2:55][CH2:54][N:53]([C:56]([C:58]2[CH:64]=[CH:63][C:61]([NH2:62])=[CH:60][CH:59]=2)=[O:57])[CH2:52][CH2:51]1)[CH3:49]>CN(C=O)C>[CH3:15][C:64]1[CH:63]=[C:61]([NH:62][C:11]([CH:10]([NH:9][C:7]([C:5]2[S:6][C:2]([Cl:1])=[CH:3][CH:4]=2)=[O:8])[CH3:14])=[O:13])[CH:60]=[CH:59][C:58]=1[C:56]([N:53]1[CH2:52][CH2:51][N:50]([CH2:48][CH3:49])[CH2:55][CH2:54]1)=[O:57]

참가 물질

6

반응물 4

HCID 81531Diisopropylethylamine2회HCID 1132820(4-Aminophenyl)(4-ethylpiperazin-1-yl)methanoneHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 432393382-[(5-Chloro-thiophene-2-carbonyl)-amino]-propionic acid

생성물 1

HCID 686371875-chloro-thiophene-2-carboxylic acid-N-{1-[3-methyl-4-(4-ethyl-piperazin-1-yl-carbonyl)-phenylcarbamoyl]-ethyl}-amide

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

200 μl of a 0.05-molar solution of 2-[(5-chloro-thiophene-2-carbonyl)-amino]-propionic acid, which additionally contains 0.05 mol/l DIPEA, in DMF are combined with 100 μl of a 0.1-molar solution of HATU in DMF on a microtitre plate and mixed for 10 min on a shaker. Then 200 μl of a 0.05-molar solution of 4-(4-ethyl-piperazin-1-yl-carbonyl)-aniline which additionally contains 0.05 mol/l DIPEA are pipetted in and the mixture is again combined by jogging. After 16 h at 80° C. the mixture is filtered through basic aluminium oxide and washed again with DMF/methanol=9:1. Then it is evaporated down i. vac.

후처리

  1. additionmixed for 10 min on a shaker
  2. filtrationAfter 16 h at 80° C. the mixture is filtered through basic aluminium oxide
  3. washwashed again with DMF/methanol=9:1
  4. customThen it is evaporated down i

출처 및 근거

ORD 기록
ord-f7acfaafafa34177ad495bcd78f243fe
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07732466B2

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