Hydrochloric Acid → 1-Hydrazinyl-3,4-dihydroisoquinoline

HRID 436430

反応式

HRID 436430 の反応式
[NH2:1][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[CH2:5][CH2:4][N:3]=1.Cl.C(OC1C2C(=CC=CC=2)CC[N:17]=1)C.[Cl-].[NH4+].C(=O)([O-])[O-].[Na+].[Na+].NN>C(O)C>[NH:1]([C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[CH2:5][CH2:4][N:3]=1)[NH2:17]

参加物

8

反応物 6

HCID 313Hydrochloric AcidHCID 9321HydrazineHCID 10340Sodium CarbonateHCID 25517Ammonium ChlorideHCID 97938243,4-Dihydro-isoquinolin-1-ylamineHCID 123490381-Ethoxy-3,4-dihydroisoquinoline

生成物 1

HCID 123490411-Hydrazinyl-3,4-dihydroisoquinoline

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
25 °C

実験手順

A mixture of 1-amino-3,4-dihydroisoquinoline (VI: R=R'=Y=Y'=Z=Z'=H) hydrochloride (m.p. 133°-134° C., 0.5 g.), prepared from 1-ethoxy-3,4-dihydroisoquinoline and ammonium chloride, sodium carbonate (0.38 g.), hydrazine (0.41 g.) and ethanol (15 ml.) was stirred (at 25° C.). The mixture was filtered. An ether solution of the crystals which separated from the filtrate on chilling was washed with water, dried and filtered. Concentration of the filtrate and crystallization of the residue from ether afforded 1-hydrazino-3,4-dihydroisoquinoline (0.44 g.).

後処理

  1. filtrationThe mixture was filtered
  2. customAn ether solution of the crystals which separated from the filtrate
  3. temperatureon chilling
  4. washwas washed with water
  5. customdried
  6. filtrationfiltered
  7. customConcentration of the filtrate and crystallization of the residue from ether

出典と根拠

ORDレコード
ord-c56f3b2b50184e3084ea8ec85fc05f53
出典データセット
uspto-grants-1977_02
特許番号
US04009170

関連ノート

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