Sodium Carbonate → HCID 20299671、化合物

HRID 1733462ノート

反応式

HRID 1733462 の反応式
[Cl:1][C:2]1[C:11]([Cl:12])=[C:10]2[C:5]([CH2:6][CH2:7][NH:8][CH2:9]2)=[CH:4][CH:3]=1.C(=O)([O-])[O-].[Na+].[Na+].Br[CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25]Br>C(O)C>[ClH:1].[ClH:1].[CH2:20]([N:8]1[CH2:7][CH2:6][C:5]2[C:10](=[C:11]([Cl:12])[C:2]([Cl:1])=[CH:3][CH:4]=2)[CH2:9]1)[CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][N:8]1[CH2:7][CH2:6][C:5]2[C:10](=[C:11]([Cl:12])[C:2]([Cl:1])=[CH:3][CH:4]=2)[CH2:9]1

参加物

5

反応物 3

HCID 10340Sodium CarbonateHCID 123681,6-DibromohexaneHCID 123920Isoquinoline, 7,8-dichloro-1,2,3,4-tetrahydro-

生成物 1

HCID 20299671HCID 20299671、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A suspension of 2.38 g. (10 mmol) of 7,8-dichloro-1,2,3,4-tetrahydroisoquinoline and 3.18 g. (30 mmol) of sodium carbonate in 50 ml. of absolute ethanol were refluxed for 5 minutes. To this suspension was added 1.22 g. (5 mmol) of 1,6-dibromohexane and the mixture refluxed overnight. The reaction was cooled and after standing for 36 hours was filtered of solid precipitate. The resulting solid was suspended in 100 ml. of ethyl acetate and treated with 1 g. of magnesium sulfate. The mixture was filtered and the filtrate treated with 10 ml. of ethereal hydrochloric acid. The resulting precipitate was removed by filtration, washed with ether and dried to give 2,2'-hexylene-bis(7,8-dichloro-1,2,3,4-tetrahydroisoquinoline)dihydrochloride having a melting point of 308°-311° C.

後処理

  1. additionA suspension of 2.38 g
  2. additionTo this suspension was added 1.22 g
  3. temperatureThe reaction was cooled
  4. filtrationwas filtered of solid precipitate
  5. additionof ethyl acetate and treated with 1 g
  6. filtrationThe mixture was filtered
  7. additionthe filtrate treated with 10 ml
  8. customThe resulting precipitate was removed by filtration
  9. washwashed with ether
  10. customdried

出典と根拠

ORDレコード
ord-926a19c7b4f043448855d4e8ec151208
出典データセット
uspto-grants-1980_12
特許番号
US04242346

反応ノート

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