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Formaldehyde → HCID 86737413、化合物

HRID 1733461
ノート
印刷プレビュー

反応式

HRID 1733461 の反応式
[ClH:1].[Cl:2][C:3]1[C:12]([Cl:13])=[C:11]2[C:6]([CH2:7][CH2:8][NH:9][CH2:10]2)=[CH:5][CH:4]=1.C=O.C(=O)([O-])[O-].[Na+].[Na+]>O>[ClH:2].[ClH:1].[Cl:2][C:3]1[C:12]([Cl:13])=[C:11]2[C:6]([CH2:7][CH2:8][NH:9][CH2:10]2)=[CH:5][CH:4]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 712FormaldehydeHCID 10340Sodium CarbonateHCID 1239197,8-Dichloro-1,2,3,4-tetrahydroisoquinoline hydrochloride

生成物 1

HCID 86737413HCID 86737413、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A solution of 2.37 g. (10 mmol) of 7,8-dichloro-1,2,3,4-tetrahydroisoquinoline hydrochloride salt and 20 ml. of 37% formalin in 100 ml. of water was stirred in an ice bath for thirty minutes. 50 ml. of 5% sodium carbonate solution was added dropwise over 10 minutes and the resulting precipitate was removed by filtration, dissolved in 50 ml. of methylene chloride, dried over magnesium sulfate and filtered. The filtrate was treated with 25 ml. of ethereal hydrogen chloride and allowed to stand in the cold overnight. The resulting precipitate was collected, washed with ether and dried to give 2,2'-methylene-bis-(7,8-dichloro-1,2,3,4-tetrahydroisoquinoline dihydrochloride, melting point 153° C. dec.

後処理

  1. customthe resulting precipitate was removed by filtration
  2. dissolutiondissolved in 50 ml
  3. dry with materialof methylene chloride, dried over magnesium sulfate
  4. filtrationfiltered
  5. additionThe filtrate was treated with 25 ml
  6. customto stand in the cold overnight
  7. customThe resulting precipitate was collected
  8. washwashed with ether
  9. customdried

出典と根拠

ORDレコード
ord-6dc9e655dac44bfb99ea54f7be581aa0
出典データセット
uspto-grants-1980_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04242346

反応ノート

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