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Water → HCID 59395386, 화합물

HRID 1097733
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HRID 1097733 반응식
[Cl:1][C:2]1[NH:10][C:9]2[C:8](=[O:11])[N:7]([CH2:12][CH2:13][CH2:14][CH2:15][C:16]([O:18]CC)=[O:17])[C:6](=[O:21])[N:5]([CH2:22][CH3:23])[C:4]=2[N:3]=1.O.[OH-].[Li+]>CO>[Cl:1][C:2]1[NH:10][C:9]2[C:8](=[O:11])[N:7]([CH2:12][CH2:13][CH2:14][CH2:15][C:16]([OH:18])=[O:17])[C:6](=[O:21])[N:5]([CH2:22][CH3:23])[C:4]=2[N:3]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 3939Lithium HydroxideHCID 59395539HCID 59395539, 화합물

생성물 1

HCID 59395386HCID 59395386, 화합물수율 95%

시약·촉매·용매 1

HCID 887Methanol용매

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온도
40 °C

실험 절차

A solution of ethyl 5-(8-chloro-3-ethyl-2,6-dioxo-2,3,6,7-tetrahydro-1H-purin-1-yl)pentanoate (2.3 g, 6.7 mmol) in methanol (75 ml) was treated with water (3 ml) and lithium hydroxide (0.481 g, 20.1 mmol) and the mixture stirred at 40° C. for 17 h. The mixture was evaporated to dryness and the residue treated with 50 ml of ethyl acetate and 50 ml of water. The 2 phases were separated and the aqueous phase adjusted to pH5 using 2M aqueous hydrochloric acid. The precipitated product was filtered off and dried to yield 5-(8-chloro-3-ethyl-2,6-dioxo-2,3,6,7-tetrahydro-1H-purin-1-yl)pentanoic acid as a white solid (1.99 g, 95%).

후처리

  1. customThe mixture was evaporated to dryness
  2. additionthe residue treated with 50 ml of ethyl acetate and 50 ml of water
  3. customThe 2 phases were separated
  4. filtrationThe precipitated product was filtered off
  5. customdried

출처 및 근거

ORD 기록
ord-a76f4d45b43c4ea198003b8ddc9d7cb4
출처 데이터셋
uspto-grants-2012_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08143264B2

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