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Hydrochloric Acid → HCID 68856131, 화합물

HRID 1986218
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HRID 1986218 반응식
[Li+].[OH-].C[O:4][C:5]([C:7]1[C:15]2[CH:14]=[C:13]([C:16]3[C:21]([Cl:22])=[CH:20][N:19]=[C:18]([NH:23][CH2:24][CH2:25][CH2:26][N:27]4[CH2:32][CH2:31][N:30]([CH3:33])[CH2:29][CH2:28]4)[N:17]=3)[S:12][C:11]=2[CH:10]=[CH:9][CH:8]=1)=[O:6].[ClH:34]>O.CO.C1COCC1>[ClH:22].[ClH:34].[ClH:22].[Cl:22][C:21]1[C:16]([C:13]2[S:12][C:11]3[CH:10]=[CH:9][CH:8]=[C:7]([C:5]([OH:6])=[O:4])[C:15]=3[CH:14]=2)=[N:17][C:18]([NH:23][CH2:24][CH2:25][CH2:26][N:27]2[CH2:28][CH2:29][N:30]([CH3:33])[CH2:31][CH2:32]2)=[N:19][CH:20]=1
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참가 물질

7

반응물 3

HCID 313Hydrochloric AcidHCID 3939Lithium HydroxideHCID 68858417HCID 68858417, 화합물

생성물 1

HCID 68856131HCID 68856131, 화합물수율 94%

시약·촉매·용매 3

HCID 887Methanol용매HCID 962Water용매
HCID 8028
Tetrahydrofuran
용매

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온도
70 °C

실험 절차

Aqueous 2 N LiOH (1.1 mL, 2.2 mmol) is added to a stirred solution of 2-{5-chloro-2-[3-(4-methylpiperazin-1-yl)-propylamino]-pyrimidin-4-yl}-benzo[b]thiophene-4-carboxylic acid methyl ester (280 mg, 0.610 mmol) in water (3 mL), MeOH (6 mL) and THF (12 mL). The mixture is heat at 70° C. for 2 hours. While at 70° C., 5 N HCl (1 mL) is added to the solution, then the solution is allowed to cool to room temperature. After concentration, the yellow solid is suspended in THF (20 mL), sonicated, filtered, and dried to give the title compound as a solid (320 mg, 94% yield).

후처리

  1. temperatureto cool to room temperature
  2. concentrationAfter concentration
  3. customsonicated
  4. filtrationfiltered
  5. customdried

출처 및 근거

ORD 기록
ord-bb17636c45834759a3c86b44c2f0a730
출처 데이터셋
uspto-grants-2009_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07547691B2

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