Picolyl chloride hydrochloride → 2-(2-Pyridiniomethyl)isothiouronium dichloride

HRID 1680188ノート

反応式

HRID 1680188 の反応式
[ClH:1].[Cl:2][CH2:3][C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][N:5]=1.[NH2:10][C:11]([NH2:13])=[S:12]>C(O)C>[ClH:2].[ClH:1].[N:5]1[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=1[CH2:3][S:12][C:11](=[NH:10])[NH2:13]

参加物

4

反応物 2

HCID 23392Picolyl chloride hydrochlorideHCID 2723790Thiourea

生成物 1

HCID 130439522-(2-Pyridiniomethyl)isothiouronium dichloride収率 94.9%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

A solution of 2-chloromethylpyridine hydrochloride (30 g) in ethanol (100 cc) at 60° C. is added dropwise, in the course of 15 minutes, to a suspension of thiourea (17.6 g) in boiling ethanol (100 cc). Boiling is maintained for 90 minutes and then, after cooling, the crystals which have appeared are filtered off, washed twice with ethanol (100 cc in total) and dried under reduced pressure (20 mm Hg) at a temperature of about 20° C., in the presence of potassium hydroxide pellets. 2-(Pyrid-2-ylmethyl)isothiourea dihydrochloride (41.7 g), melting at 220° C., is thus obtained.

後処理

  1. temperatureBoiling is maintained for 90 minutes
  2. temperatureafter cooling
  3. filtrationthe crystals which have appeared are filtered off
  4. washwashed twice with ethanol (100 cc in total)
  5. dry with materialdried under reduced pressure (20 mm Hg) at a temperature of about 20° C., in the presence of potassium hydroxide pellets

出典と根拠

ORDレコード
ord-daea576ab7c44eed96bff6c1b10dbd34
出典データセット
uspto-grants-1981_06
特許番号
US04272534

反応ノート

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