Acetic Acid → HCID 13121507, 화합물

HRID 973045

반응식

HRID 973045 반응식
[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]

참가 물질

8

반응물 4

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

생성물 1

HCID 13121507HCID 13121507, 화합물

시약·촉매·용매 3

HCID 5360545Sodium촉매HCID 702Ethanol용매2회HCID 962Water용매2회

실험 절차

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 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.).

후처리

  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 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

출처 및 근거

ORD 기록
ord-9a4da07c488849e2a62b81430e6c542a
출처 데이터셋
uspto-grants-1977_10
특허 번호
US04054656

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