Aniline → N,N-Di(6-hydroxyhexyl)aniline

HRID 2291429

反応式

HRID 2291429 の反応式
[NH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:8](=[O:11])([O-])[O-].[K+].[K+].Cl[CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][OH:21]>>[OH:21][CH2:20][CH2:19][CH2:18][CH2:17][CH2:16][CH2:15][N:1]([CH2:4][CH2:3][CH2:2][CH2:7][CH2:6][CH2:8][OH:11])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

4

反応物 3

HCID 6115AnilineHCID 11430Potassium CarbonateHCID 748286-Chloro-1-hexanol

生成物 1

HCID 21982671N,N-Di(6-hydroxyhexyl)aniline収率 127%

実験手順

A mixture of freshly distilled aniline (93 g, 1.10 mol), potassium carbonate (304 g, 2.2 mol), 6-chloro-1-hexanol (300.0 g, 2.2 mol), and 500 mL of η-butanol was heated at reflux for 82 hours under nitrogen with vigorous stirring. After cooling and filtering, the butanol was evaporated at reduced pressure to leave a tan oil. The oil was fractionally distilled in vacuo, yielding 205 g (70%) of A1 as a colorless oil, bp 195°-225° C. (0.15 nm).

後処理

  1. temperaturewas heated
  2. temperatureat reflux for 82 hours under nitrogen with vigorous stirring
  3. temperatureAfter cooling
  4. filtrationfiltering
  5. customthe butanol was evaporated at reduced pressure
  6. customto leave a tan oil
  7. distillationThe oil was fractionally distilled in vacuo

出典と根拠

ORDレコード
ord-405f877d462048c0833a911c51b535a3
出典データセット
uspto-grants-1989_01
特許番号
US04796971

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