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Citric Acid → HCID 178425833, 화합물

HRID 1046461
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HRID 1046461 반응식
C[O:2][C:3]([C:5]1[S:6][C:7]([C:27]#[C:28][C:29]([CH3:32])([CH3:31])[CH3:30])=[CH:8][C:9]=1[N:10]([C@H:20]1[CH2:25][CH2:24][C@H:23]([OH:26])[CH2:22][CH2:21]1)[C:11]([CH:13]1[CH2:18][CH2:17][C:16]([CH3:19])=[CH:15][CH2:14]1)=[O:12])=[O:4].[CH3:33][N:34]([CH2:36][C:37]1[CH:42]=[CH:41][N:40]=[C:39](F)[CH:38]=1)[CH3:35].[H-].[Na+].C(O)(=O)CC(CC(O)=O)(C(O)=O)O>CN(C=O)C.O>[CH3:33][N:34]([CH2:36][C:37]1[CH:42]=[CH:41][N:40]=[C:39]([O:26][C@H:23]2[CH2:24][CH2:25][C@H:20]([N:10]([C:11]([CH:13]3[CH2:18][CH2:17][C:16]([CH3:19])=[CH:15][CH2:14]3)=[O:12])[C:9]3[CH:8]=[C:7]([C:27]#[C:28][C:29]([CH3:30])([CH3:31])[CH3:32])[S:6][C:5]=3[C:3]([OH:2])=[O:4])[CH2:21][CH2:22]2)[CH:38]=1)[CH3:35]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 311Citric AcidHCID 24758Sodium hydrideHCID 58113973HCID 58113973, 화합물HCID 178499326HCID 178499326, 화합물

생성물 1

HCID 178425833HCID 178425833, 화합물수율 35%

시약·촉매·용매 2

HCID 962Water용매
HCID 6228
Dimethylformamide
용매

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온도
90 °C

실험 절차

5-(3,3-Dimethyl-but-1-ynyl)-3-[(4-hydroxy-trans-cyclohexyl)-(4-methyl-cyclohex-3-enecarbonyl)-amino]-thiophene-2-carboxylic acid methyl ester (40 mg, 0.088 mmol) and (N,N-dimethyl)-(2-fluoro-pyridin-4-ylmethyl)amine (84 mg, 0.55 mmol) in DMF (1 mL) were treated with sodium hydride (22 mg, 60% oil dispersion, 0.55 mmol). After the bubbling slowed, the reaction mixture was sealed and heated by microwave (90° C.) for 70 min. The reaction mixture was treated with 10% citric acid (2-3 mL) followed by water (2-3 mL). The organics were extracted twice with ethyl acetate, dried over sodium sulfate, filtered and concentrated. The residue was purified by reverse phase HPLC to give the Compound 337, 18 mg (35% yield): MS (m/z): 578.0 [M+H]+; HPLC retention time 3.53 min (2-98% acetonitrile:water with 0.05% trifluoroacetic acid).

후처리

  1. customthe reaction mixture was sealed
  2. extractionThe organics were extracted twice with ethyl acetate
  3. dry with materialdried over sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customThe residue was purified by reverse phase HPLC

출처 및 근거

ORD 기록
ord-6d47c877498540bc948e346173f92c75
출처 데이터셋
uspto-grants-2013_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08569302B2

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