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1,2-Dichloroethane → HCID 58345391, 화합물

HRID 1877992
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HRID 1877992 반응식
O=O.C(Cl)CCl.C1C=CC2N(O)N=NC=2C=1.[CH:17]([OH:19])=O.[Cl:20][C:21]1[CH:22]=[C:23]([N:27]2[C:31]([C:32]3[CH:37]=[CH:36][CH:35]=[C:34]([S:38][C:39]([F:42])([F:41])[F:40])[CH:33]=3)=[CH:30][C:29]([C:43]([N:45]3[CH2:50][CH2:49][NH:48][CH2:47][CH2:46]3)=[O:44])=[N:28]2)[CH:24]=[CH:25][CH:26]=1.ClC1C=C(N2C(C3C=CC=C(SC(F)(F)F)C=3)=CC(C(O)=O)=N2)C=CC=1.N1CCNCC1>CN(C=O)C>[Cl:20][C:21]1[CH:22]=[C:23]([N:27]2[C:31]([C:32]3[CH:37]=[CH:36][CH:35]=[C:34]([S:38][C:39]([F:41])([F:42])[F:40])[CH:33]=3)=[CH:30][C:29]([C:43]([N:45]3[CH2:50][CH2:49][N:48]([CH:17]=[O:19])[CH2:47][CH2:46]3)=[O:44])=[N:28]2)[CH:24]=[CH:25][CH:26]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

9

반응물 7

HCID 111,2-DichloroethaneHCID 284Formic AcidHCID 977OxygenHCID 4837PiperazineHCID 757711-HydroxybenzotriazoleHCID 58345430HCID 58345430, 화합물HCID 67312911HCID 67312911, 화합물

생성물 1

HCID 58345391
HCID 58345391, 화합물
수율 42%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

Under exclusion of oxygen, 17.2 mg (0.09 mmol) of EDC and 11.7 mg (0.09 mmol) of HOBt and 8.3 mg (0.18 mmol) of formic acid are added to a solution of 35.0 mg (0.07 mmol) of 1-{[1-(3-chlorophenyl)-5-(3-trifluoromethylthiophenyl)-1H-pyrazol-3-yl]carbonyl}piperazine, prepared from the compound of example 8A and piperazine in analogy to example 1, in 1 ml DMF, and the mixture is stirred for 72 hours at room temperature. The reaction mixture is separated by preparative HPLC. 15.7 mg (42% yield of theory) of product are obtained.

후처리

  1. customThe reaction mixture is separated by preparative HPLC
  2. custom15.7 mg (42% yield of theory) of product are obtained

출처 및 근거

ORD 기록
ord-0daee40b48be43d1a6f1c3eb62ca51c0
출처 데이터셋
uspto-grants-2012_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08314089B2

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