Cyanamide → HCID 178512274、化合物

HRID 864489

反応式

HRID 864489 の反応式
[O:1]([CH2:8][CH2:9][CH2:10][CH2:11][NH:12][C:13]([NH:15][C:16]1[CH:17]=[N:18][CH:19]=[CH:20][CH:21]=1)=S)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[N:22]#[C:23][NH2:24].C1(N=C=NC2CCCCC2)CCCCC1.C1(NC(NC2CCCCC2)=S)CCCCC1>C(#N)C.C(N(CC)CC)C>[C:23]([NH:24][C:13]([NH:12][CH2:11][CH2:10][CH2:9][CH2:8][O:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1)=[N:15][C:16]1[CH:17]=[N:18][CH:19]=[CH:20][CH:21]=1)#[N:22]

参加物

7

反応物 4

HCID 9864CyanamideHCID 10868DicyclohexylcarbodiimideHCID 727200DicyclohexylthioureaHCID 21467376N-(4-Phenoxybutyl)-N'-3-pyridylthiourea

生成物 1

HCID 178512274HCID 178512274、化合物

試薬・触媒・溶媒 2

HCID 6342Acetonitrile溶媒HCID 8471Triethylamine溶媒

実験手順

N-(4-Phenoxybutyl)-N'-3-pyridylthiourea (1.41 g) was dissolved in acetonitrile (10 ml), and cyanamide (400 mg), N,N'dicyclohexylcarbodiimide (1.95 g) and triethylamine (0.08 ml) were added. The mixture was stirred for 3 days at room temperature, when it was filtered, washed with acetonitrile, and ether to yield a solid mixture of the crude product and N,N'-dicyclohexylthiourea. The pure compound was obtained by extracting the mixture with 0.5N hydrochloric acid (16 ml), filtering and re-precipitation by addition of 9N sodium hydroxide to the filtrate.

後処理

  1. filtrationwhen it was filtered
  2. washwashed with acetonitrile, and ether
  3. customto yield
  4. customThe pure compound was obtained
  5. extractionby extracting the mixture with 0.5N hydrochloric acid (16 ml)
  6. filtrationfiltering
  7. customre-precipitation
  8. additionby addition of 9N sodium hydroxide to the filtrate

出典と根拠

ORDレコード
ord-002fafce572d40b990540ea766675467
出典データセット
uspto-grants-1996_10
特許番号
US05563160

関連ノート

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