Acetic Acid → HCID 13121507、化合物

HRID 237124

反応式

HRID 237124 の反応式
[NH2:1][C:2]1[S:6][C:5]2[CH2:7][CH2:8][CH2:9][CH2:10][C:4]=2[C:3]=1[C:11]([NH2:13])=[O:12].[O-:14]CC.[Na+].[C:18]([OH:21])(=[O:20])[CH3:19].Cl>[Na].O.C(O)C>[NH2:13][C:11]([C:3]1[C:4]2[CH2:10][CH2:9][CH2:8][CH2:7][C:5]=2[S:6][C:2]=1[NH:1][C:19](=[O:14])[C:18]([OH:21])=[O:20])=[O:12]

参加物

8

反応物 4

HCID 176Acetic AcidHCID 313Hydrochloric AcidHCID 2902232-Amino-4,5,6,7-tetrahydro-1-benzothiophene-3-carboxamideHCID 2723922Sodium ethoxide

生成物 1

HCID 13121507HCID 13121507、化合物

試薬・触媒・溶媒 3

HCID 5360545Sodium触媒HCID 702Ethanol溶媒2 回HCID 962Water溶媒2 回

実験手順

A suspension of 392 g. (2.0 mole) of 2-amino-4,5,6,7-tetrahydrobenzo[b]thiophene-3-carboxamide and 321.2 g. (2.2 mole) of diethyl oxylate in 5 l. of absolute ethanol is added to a solution of sodium ethoxide, prepared from 50.6 g. (2.2 g. atoms) of sodium, in 2 l. of absolute ethanol under nitrogen. The mixture is stirred with heating at the reflux temperature for 6 hrs. and then refrigerated overnight. It is then diluted with stirring to 15 l. with cool water. A finely divided precipitate forms which is removed by filtration. The filtrate is carefully acidified with 150 g. (2.5 mole) of acetic acid dissolved in 350 ml. of water. The resulting product which precipitates is collected on a filter, washed with water, and air dried to yield 194.6 g. (0.7 mole) of the product of Procedure 2. The filtrate is acidified to pH 2 with concentrated hydrochloric acid and the resulting precipitate is collected on a filter, washed with water and air dried to give 264.8 g. (0.99 mole) of the desired product. A portion thereof weighing 25 g. is recrystallized from 1.4 l. of dioxane, yield 18.2 g., m.p. 223.5°-224.5° C. (dec.).

後処理

  1. additionA suspension of 392 g
  2. customprepared from 50.6 g
  3. temperaturewith heating at the reflux temperature for 6 hrs
  4. customrefrigerated overnight
  5. additionIt is then diluted
  6. stirringwith stirring to 15 l
  7. customA finely divided precipitate forms which is removed by filtration
  8. customThe resulting product which precipitates
  9. customis collected on a filter
  10. washwashed with water, and air
  11. customdried
  12. customto yield 194.6 g
  13. customthe resulting precipitate is collected on a filter
  14. washwashed with water and air
  15. customdried
  16. customto give 264.8 g

出典と根拠

ORDレコード
ord-4f12f4109b654e34810204d18727d3c9
出典データセット
uspto-grants-1979_06
特許番号
US04159377

関連ノート

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