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Lithium Hydroxide → 4-(5-Cyclopropylmethoxy-1,3-benzodioxol-4-yl)-5H-pyrrolo[3,2-d]pyrimidine-7-carboxylic acid

HRID 2093868
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HRID 2093868 반응식
C([O:3][C:4]([C:6]1[C:10]2[N:11]=[CH:12][N:13]=[C:14]([C:15]3[C:23]4[O:22][CH2:21][O:20][C:19]=4[CH:18]=[CH:17][C:16]=3[O:24][CH2:25][CH:26]3[CH2:28][CH2:27]3)[C:9]=2[NH:8][CH:7]=1)=[O:5])C.[Li+].[OH-]>O1CCOCC1.O>[CH:26]1([CH2:25][O:24][C:16]2[CH:17]=[CH:18][C:19]3[O:20][CH2:21][O:22][C:23]=3[C:15]=2[C:14]2[C:9]3[NH:8][CH:7]=[C:6]([C:4]([OH:5])=[O:3])[C:10]=3[N:11]=[CH:12][N:13]=2)[CH2:27][CH2:28]1
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참가 물질

5

반응물 2

HCID 3939Lithium HydroxideHCID 668669824-(5-Cyclopropylmethoxy-1,3-benzodioxol-4-yl)-5H-pyrrolo[3,2-d]pyrimidine-7-carboxylic acid ethyl ester

생성물 1

HCID 668660154-(5-Cyclopropylmethoxy-1,3-benzodioxol-4-yl)-5H-pyrrolo[3,2-d]pyrimidine-7-carboxylic acid수율 93.1%

시약·촉매·용매 2

HCID 962Water용매HCID 312751,4-Dioxane
용매

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온도
100 °C

실험 절차

4-(5-Cyclopropylmethoxy-1,3-benzodioxol-4-yl)-5H-pyrrolo[3,2-d]pyrimidine-7-carboxylic acid ethyl ester (9.53 g; 25.0 mmol) from example A48 is suspended in dioxane (170 mL) and water (100 mL). After addition of LiOH (2.99 g; 125.0 mmol) the reaction mixture is stirred at 100° C. over night. The resulting solution is evaporated to dryness. The residue is dissolved in hot (60-90° C.) water (250 mL) and pH is adjusted to 2-3 by addition of 2M citric acid while still hot. After cooling to ambient temperature the precipitated product is collected by suction filtration, washed with water, ethanol and dried in high vacuo at 50° C. to yield 8.22 g of the title compound as pale yellow solid.

후처리

  1. customThe resulting solution is evaporated to dryness
  2. dissolutionThe residue is dissolved in hot (60-90° C.) water (250 mL) and pH
  3. additionis adjusted to 2-3 by addition of 2M citric acid while still hot
  4. temperatureAfter cooling to ambient temperature the precipitated product
  5. filtrationis collected by suction filtration
  6. washwashed with water, ethanol
  7. customdried in high vacuo at 50° C.

출처 및 근거

ORD 기록
ord-2d2bbfde5aea4cc09927c64ad55ff3b0
출처 데이터셋
uspto-grants-2013_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08445501B2

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