Hydrochloric Acid → HCID 20183530, 화합물

HRID 255509노트

반응식

HRID 255509 반응식
[OH:1][C:2]1[C:10]([CH2:11][CH2:12][CH3:13])=[C:9]2[C:5]([CH:6]=[C:7]([C:14]([O:16]CC)=[O:15])[NH:8]2)=[CH:4][CH:3]=1.[C:19]([C:25](OC)=[O:26])#[C:20][C:21]([O:23]C)=[O:22].[OH-].[Na+].Cl>C(O)C.O>[O:26]=[C:25]1[C:3]2[CH:4]=[C:5]3[C:9](=[C:10]([CH2:11][CH2:12][CH3:13])[C:2]=2[O:1][C:20]([C:21]([OH:23])=[O:22])=[CH:19]1)[NH:8][C:7]([C:14]([OH:16])=[O:15])=[CH:6]3

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 12980Dimethyl acetylenedicarboxylateHCID 14798Sodium HydroxideHCID 20183534HCID 20183534, 화합물

생성물 1

HCID 20183530HCID 20183530, 화합물

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

The product of step (c) (0.6 g, 0.0024 M), dimethyl acetylene dicarboxylate (0.33 ml, 0.0027 M) and "Triton B" (2 drops) were heated under reflux for 6 hours in dry ethanol (10 ml). The reaction mixture was cooled, NaOH (0.6 g, 14.6 mmol) in water (6 ml) was added and refluxing continued for 1 hour. The whole was cooled, poured into dil. HCl, extracted into ethyl acetate and washed with brine before drying over MgSO4 and evaporating to dryness to yield the sub-title compound as a pale yellow solid, 0.7 g, (86%).

후처리

  1. temperatureThe reaction mixture was cooled
  2. temperaturerefluxing
  3. temperatureThe whole was cooled
  4. extractionextracted into ethyl acetate
  5. washwashed with brine
  6. dry with materialbefore drying over MgSO4
  7. customevaporating to dryness

출처 및 근거

ORD 기록
ord-e81a767ea03246699b9899c48f4b1a17
출처 데이터셋
uspto-grants-1987_10
특허 번호
US04698345

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