Formic Acid → HCID 13518767、化合物

HRID 370447ノート

反応式

HRID 370447 の反応式
[Cl:1][C:2]1[C:11]2[CH:10]3[CH2:12][CH2:13][CH:7]([CH2:8][CH2:9]3)[C:6]=2[C:5]([NH:14][NH2:15])=[N:4][N:3]=1.[CH:16](O)=O>>[Cl:1][C:2]1[C:11]2[CH:10]3[CH2:9][CH2:8][CH:7]([CH2:13][CH2:12]3)[C:6]=2[C:5]2=[N:14][N:15]=[CH:16][N:4]2[N:3]=1

参加物

3

反応物 2

HCID 284Formic AcidHCID 110205581-Chloro-4-hydrazinyl-5,6,7,8-tetrahydro-5,8-ethanophthalazine

生成物 1

HCID 13518767HCID 13518767、化合物収率 88%

実験手順

1-Chloro-4-hydrazino-5,6,7,8-tetrahydro-5,8-ethanophthalazine (2.5 grams, 0.111 mol) was mixed with 150 milliliters of formic acid. The mixture was heated at the boiling temperature under reflux for 2 hours, then evaporated to dryness. The residue was triturated with saturated aqueous sodium bicarbonate. The resulting white solid was collected, washed with water and air dried to yield 23.0 grams (88% yield) of 6-chloro-7,8,9,10-tetrahydro-7,10-ethano(1,2,4)triazolo[3,4-a]phthalazine, melting at 137°-140° C. After recrystallization from a mixture of benzene and hexane the purified product melted at 140.5°-141° C. Infrared spectroscopy and elemental analysis confirmed the designated structure.

後処理

  1. temperatureThe mixture was heated at the boiling temperature
  2. temperatureunder reflux for 2 hours
  3. customevaporated to dryness
  4. customThe residue was triturated with saturated aqueous sodium bicarbonate
  5. customThe resulting white solid was collected
  6. washwashed with water and air
  7. customdried

出典と根拠

ORDレコード
ord-96d163f016d949989ca8a84675001844
出典データセット
uspto-grants-1985_07
特許番号
US04526890

反応ノート

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