Hydrochloric Acid → HCID 20183530、化合物

HRID 255509ノート

反応式

HRID 255509 の反応式
[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

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 12980Dimethyl acetylenedicarboxylateHCID 14798Sodium HydroxideHCID 20183534HCID 20183534、化合物

生成物 1

HCID 20183530HCID 20183530、化合物

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-e81a767ea03246699b9899c48f4b1a17
出典データセット
uspto-grants-1987_10
特許番号
US04698345

反応ノート

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