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Pyridine → 2,3-Dihydroxypropyl-4-hexadecylaminobenzamide

HRID 2163776
ノート
印刷プレビュー

反応式

HRID 2163776 の反応式
Cl.[CH2:2]([NH:18][C:19]1[CH:27]=[CH:26][C:22]([C:23]([OH:25])=O)=[CH:21][CH:20]=1)[CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH3:17].C(Cl)Cl.S(Cl)(Cl)=O.N[CH2:36][CH:37]([OH:40])[CH2:38][OH:39].[N:41]1C=CC=CC=1>CN(C)C1C=CN=CC=1.C(COC)OC>[OH:40][CH:37]([CH2:38][OH:39])[CH2:36][C:21]1[CH:20]=[C:19]([NH:18][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH3:17])[CH:27]=[CH:26][C:22]=1[C:23]([NH2:41])=[O:25]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 1049PyridineHCID 6344DichloromethaneHCID 24386Thionyl ChlorideHCID 735613-Amino-1,2-propanediolHCID 70506019HCID 70506019、化合物

生成物 1

HCID 204373882,3-Dihydroxypropyl-4-hexadecylaminobenzamide

試薬・触媒・溶媒 2

HCID 14284
4-(Dimethylamino)pyridine
触媒
HCID 80711,2-Dimethoxyethane溶媒

実験手順

A slurry of 8.0 g. of 4-(hexadecylamino)benzoic acid hydrochloride in 175 ml. of CH2Cl2 and 50 ml. of glyme containing 10 ml. of thionyl chloride was heated at reflux for 2 hours. The clear solution was concentrated in vacuo giving 9.5 g. of an amber oil. This oil was diluted with 50 ml. of pyridine containing 0.1 g. of 4-dimethylaminopyridine and 9.1 g. of 3-amino-1,2-propandiol. The reaction was stirred for two days at room temperature. The solution was partitioned between ether and water. The water phase was extracted twice more with 100 ml. of chloroform and ether. The combined organic layer was extracted with water, dried over MgSO4 and evaporated to a tacky solid. The solid was recrystallized from acetone-water and a second time from benzene. A small sample was recrystallized from acetonitrile, m.p. 121°-122° C.

後処理

  1. temperatureat reflux for 2 hours
  2. concentrationThe clear solution was concentrated in vacuo
  3. customgiving 9.5 g
  4. additionThis oil was diluted with 50 ml
  5. customThe solution was partitioned between ether and water
  6. extractionThe water phase was extracted twice more with 100 ml
  7. extractionThe combined organic layer was extracted with water
  8. dry with materialdried over MgSO4
  9. customevaporated to a tacky solid
  10. customThe solid was recrystallized from acetone-water
  11. customA small sample was recrystallized from acetonitrile, m.p. 121°-122° C.

出典と根拠

ORDレコード
ord-e56e52f8e439426ca5dc7ce3590f707e
出典データセット
uspto-grants-1979_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04136256

反応ノート

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