Triethylamine → 3-(4-Benzylpiperazin-1-yl)propanethiol dihydrochloride

HRID 2290847

反応式

HRID 2290847 の反応式
NC(N)=[S:3].[ClH:5].Cl.[CH2:7]([N:14]1[CH2:19][CH2:18][N:17]([CH2:20][CH2:21][CH2:22][Cl:23])[CH2:16][CH2:15]1)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.C(N(CC)CC)C.[OH-].[Na+]>O.C(O)C>[ClH:23].[ClH:5].[CH2:7]([N:14]1[CH2:19][CH2:18][N:17]([CH2:20][CH2:21][CH2:22][SH:3])[CH2:16][CH2:15]1)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1

参加物

7

反応物 4

HCID 8471TriethylamineHCID 14798Sodium HydroxideHCID 2723790ThioureaHCID 13731110Benzyl-4-(3-chloropropyl)piperazine dihydrochloride

生成物 1

HCID 137311143-(4-Benzylpiperazin-1-yl)propanethiol dihydrochloride収率 78%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

15 g of thiourea were added to a solution of 35 g of 1-benzyl-4-(3-chloropropyl)piperazine dihydrochloride, 20 g of triethylamine and 250 ml of reagent ethanol, and the mixture was refluxed for 8 hours. After the addition of a solution of 10 g of sodium hydroxide in 50 ml of water, the resulting mixture was refluxed for 4 additional hours. The ethanol was removed in vacuo, and water added to the residue which was extracted with methylene chloride, dried (sodium sulfate), and the salt was precipitated with ethereal hydrochloric acid to give 25.1 g (78% of theory) of 3-(4-benzylpiperazin-1-yl)propanethiol dihydrochloride as a white crystalline solid, M.p. 270°-273° C. (dec.).

後処理

  1. temperaturethe mixture was refluxed for 8 hours
  2. temperaturethe resulting mixture was refluxed for 4 additional hours
  3. customThe ethanol was removed in vacuo, and water
  4. additionadded to the residue which
  5. extractionwas extracted with methylene chloride
  6. dry with materialdried (sodium sulfate)
  7. customthe salt was precipitated with ethereal hydrochloric acid

出典と根拠

ORDレコード
ord-bd16d46356f54e52ade0e7d429a9301d
出典データセット
uspto-grants-1986_10
特許番号
US04618677

関連ノート

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