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Ethyl Acetate → HCID 59596400, 화합물

HRID 2264581
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HRID 2264581 반응식
[F:1][C:2]([F:33])([F:32])[C:3]1[CH:4]=[C:5]([NH:17][C:18]([N:20]2[CH2:26][CH2:25][CH2:24][CH2:23][C:22]3[CH:27]=[C:28]([OH:31])[CH:29]=[CH:30][C:21]2=3)=[O:19])[CH:6]=[CH:7][C:8]=1[CH2:9][N:10]1[CH2:15][CH2:14][N:13]([CH3:16])[CH2:12][CH2:11]1.[NH2:34][C:35]1[N:40]=[C:39](Cl)[CH:38]=[C:37]([Cl:42])[N:36]=1.[OH-].[Na+].CCOC(C)=O>CC(C)=O.O.CN1C(=O)N(C)CC1>[F:33][C:2]([F:32])([F:1])[C:3]1[CH:4]=[C:5]([NH:17][C:18]([N:20]2[CH2:26][CH2:25][CH2:24][CH2:23][C:22]3[CH:27]=[C:28]([O:31][C:39]4[CH:38]=[C:37]([Cl:42])[N:36]=[C:35]([NH2:34])[N:40]=4)[CH:29]=[CH:30][C:21]2=3)=[O:19])[CH:6]=[CH:7][C:8]=1[CH2:9][N:10]1[CH2:11][CH2:12][N:13]([CH3:16])[CH2:14][CH2:15]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 8857Ethyl AcetateHCID 14798Sodium HydroxideHCID 655222-Amino-4,6-dichloropyrimidineHCID 86618288HCID 86618288, 화합물

생성물 1

HCID 59596400HCID 59596400, 화합물

시약·촉매·용매 3

HCID 180Acetone용매
HCID 962
Water
용매
2회
HCID 66611,3-Dimethyl-2-imidazolidinone용매

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온도
60 °C

실험 절차

A mixture of 300 mg (0.65 mMol) of 7-hydroxy-2,3,4,5-tetrahydro-benzo[b]azepine-1-carboxylic acid [3-trifluoromethyl-4-(4-methylpiperazin-1-ylmethyl)-phenyl]-amide (Step 12.2), 106 mg (0.65 mMol) 2-amino-4,6-dichloro-pyrimidine and 26 mg (0.65 mMol) NaOH in 2 ml acetone, 2 ml H2O and 1.2 ml DMEU is stirred at 60° C. for 12 h. Then the suspension is dissolved by addition of water and EtOAc, the aqueous phase separated off and extracted twice with EtOAc. The organic layers are washed with water and brine, dried (Na2SO4) and concentrated. Reversed phase MPLC (Gilson system) gives the title compound: MS: [M+1]+=590/592; HPLC: AtRet=12.7.

후처리

  1. customthe aqueous phase separated off
  2. extractionextracted twice with EtOAc
  3. washThe organic layers are washed with water and brine
  4. dry with materialdried (Na2SO4)
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-9fb9e29aacc54581babd47fdba235641
출처 데이터셋
uspto-grants-2010_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07855215B2

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