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Methanol → HCID 178499646, 화합물

HRID 1031762
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HRID 1031762 반응식
[NH:1]1[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[C:3]([CH2:10][C:11]([OH:13])=[O:12])=[N:2]1.[CH3:14]O>S(=O)(=O)(O)O>[NH:1]1[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[C:3]([CH2:10][C:11]([O:13][CH3:14])=[O:12])=[N:2]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 887MethanolHCID 178525248HCID 178525248, 화합물

생성물 1

HCID 178499646HCID 178499646, 화합물

시약·촉매·용매 1

HCID 1118Sulfuric Acid촉매

실험 절차

A solution of 1H-indazole-3-acetic acid (1.0 g) prepared according to J. Am. Chem. Soc., 79, 5245 (1957), in methanol (30 ml) containing five drops of concentrated sulfuric acid was refluxed for 8 hours. The reaction mixture was then concentrated to a low volume and diluted with ethyl acetate (20 ml). The organic layer was washed with water (2×10 ml) and then with sodium bicarbonate solution (10 ml, 10%). The ethyl acetate layer was collected and then dried to obtain the title compound (yield: 0.8g; m.p. 146° C.).

후처리

  1. temperaturewas refluxed for 8 hours
  2. concentrationThe reaction mixture was then concentrated to a low volume
  3. additiondiluted with ethyl acetate (20 ml)
  4. washThe organic layer was washed with water (2×10 ml)
  5. customThe ethyl acetate layer was collected
  6. customdried

출처 및 근거

ORD 기록
ord-101dd6dfffea4ab89af305bcc24d10ef
출처 데이터셋
uspto-grants-1990_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04954629

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