Butyl isocyanate → 4-Isothiocyanatophenyl butylcarbamate

HRID 1974224

反応式

HRID 1974224 の反応式
[OH:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]=[C:9]=[S:10])=[CH:4][CH:3]=1.[CH2:11]([N:15]=[C:16]=[O:17])[CH2:12][CH2:13][CH3:14].C([O-])(=O)CCCCCCCCCCC.C([O-])(=O)CCCCCCCCCCC.C([Sn+2]CCCC)CCC>C(N(CC)CC)C.C1C=CC=CC=1>[CH2:11]([NH:15][C:16]([O:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]=[C:9]=[S:10])=[CH:4][CH:3]=1)=[O:17])[CH2:12][CH2:13][CH3:14]

参加物

6

反応物 3

HCID 8110Butyl isocyanateHCID 102208Phenol, 4-isothiocyanato-HCID 9809426Di-n-butyldilauryltin

生成物 1

HCID 214890094-Isothiocyanatophenyl butylcarbamate

試薬・触媒・溶媒 2

HCID 8471Triethylamine触媒HCID 241Benzene溶媒

実験手順

Three and eight-tenths grams (3.8 g.) (0.025 m.) of p-hydroxyphenylisothiocyanate was mixed with 2.5 g. (0.025 m.) of n-butylisocyanate in 50 mls. of benzene. To this mixture was added 3 drops each of triethylamine and dibutyltin dilaurate, and the mixture was allowed to stand at ambient temperature over night. After refluxing on the steam-bath for thirty minutes, the solvent was removed under vacuum by means of a rotary evaporator. The residue was slurried in n-hexane, filtered and air dried. There was obtained 5.4 grams of solid, m.p. 99°-102° C. The structure was confirmed by I.R.

後処理

  1. waitto stand at ambient temperature over night
  2. temperatureAfter refluxing on the steam-bath for thirty minutes
  3. customthe solvent was removed under vacuum by means of a rotary evaporator
  4. filtrationfiltered
  5. customair dried

出典と根拠

ORDレコード
ord-d0fa6f81caed4614be214d4a11910119
出典データセット
uspto-grants-1976_12
特許番号
US04000253

関連ノート

読み込み中…