HCID 12533738、化合物 → HCID 10536971、化合物

HRID 434706ノート

反応式

HRID 434706 の反応式
O[NH:2][CH:3]1[C:9]2[CH:10]=[CH:11][CH:12]=[CH:13][C:8]=2[C:7](=[CH2:14])[C:6]2[CH:15]=[CH:16][CH:17]=[CH:18][C:5]=2[CH2:4]1>C(O)(=O)C.[Zn]>[NH2:2][CH:3]1[C:9]2[CH:10]=[CH:11][CH:12]=[CH:13][C:8]=2[C:7](=[CH2:14])[C:6]2[CH:15]=[CH:16][CH:17]=[CH:18][C:5]=2[CH2:4]1

参加物

4

反応物 1

HCID 12533738HCID 12533738、化合物

生成物 1

HCID 10536971HCID 10536971、化合物

試薬・触媒・溶媒 2

HCID 23994Zinc触媒HCID 176Acetic Acid溶媒

実験手順

To a stirred slurry of zinc dust (0.9 g, 0.138 mole) in 100 ml of glacial acetic acid stirred in an oil bath at 65° was added 10-hydroxyamino-5-methylene-10,11-dihydro-5H-dibenzo[a,d]cycloheptene (10 g, 42 mmole). The mixture was stirred in the oil bath for 2 hours, cooled, and quenched in 500 ml of water. The mixture was made basic with concentrated ammonia, then extracted with ether. The combined ether layers were washed with water, dried over sodium sulfate, filtered, and evaporated to dryness in vacuo. The residue was recrystallized from hexane to give 7.8 g, m.p. 84.5°-86.5°.

後処理

  1. temperaturecooled
  2. customquenched in 500 ml of water
  3. extractionextracted with ether
  4. washThe combined ether layers were washed with water
  5. dry with materialdried over sodium sulfate
  6. filtrationfiltered
  7. customevaporated to dryness in vacuo
  8. customThe residue was recrystallized from hexane
  9. customto give 7.8 g, m.p. 84.5°-86.5°

出典と根拠

ORDレコード
ord-066f1b2ff0604f3ebf83b6c8a6da7bd1
出典データセット
uspto-grants-1983_08
特許番号
US04399141

反応ノート

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