Hydrochloric Acid → 8-Chloro-2,3-dihydro-1,4-benzodioxin-5-carboxylic acid

HRID 1660028노트

반응식

HRID 1660028 반응식
N[C:2]1[C:7]2[O:8][CH2:9][CH2:10][O:11][C:6]=2[C:5]([C:12]([OH:14])=[O:13])=[CH:4][CH:3]=1.N([O-])=O.[Na+].[ClH:19]>O>[Cl:19][C:2]1[C:7]2[O:8][CH2:9][CH2:10][O:11][C:6]=2[C:5]([C:12]([OH:14])=[O:13])=[CH:4][CH:3]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric Acid2회HCID 211934708-Amino-2,3-dihydrobenzo[b][1,4]dioxine-5-carboxylic acidHCID 23668193Sodium Nitrite

생성물 1

HCID 233670468-Chloro-2,3-dihydro-1,4-benzodioxin-5-carboxylic acid수율 62%

시약·촉매·용매 1

HCID 962Water용매2회

반응 조건

온도
40 °C

실험 절차

29.3 g of 8-amino-1,4-benzodioxane-5-carboxylic acid, 120 ml of water and 30 ml of hydrochloric acid were introduced into a balloon flask provided with an agitator and a thermometer. The mixture was heated to 40° C. and then cooled to 5° C. and a solution of 10.5 g of sodium nitrite in 20 ml of water was added in portions with the temperature being maintained at from 5°-10° C. The mixture was agitated and then poured into a solution of 12 g of cuprous chloride in 45 ml of hydrochloric acid (d=1.18) with the temperature being maintained below 30° C. The precipitate was dried off, washed in 300 ml of water and 25 g of sodium bicarbonate. The solution was filtered and treated with hydrochloric acid. The precipitate was dried off, washed with water and dried. 20 g of 8-chloro-1,4-benzodioxane-5-carboxylic acid were obtained (M.P.: 195° C.; yield: 62%).

후처리

  1. customprovided with an agitator
  2. temperaturecooled to 5° C.
  3. temperaturebeing maintained at from 5°-10° C
  4. temperaturebeing maintained below 30° C
  5. customThe precipitate was dried off
  6. washwashed in 300 ml of water
  7. filtrationThe solution was filtered
  8. additiontreated with hydrochloric acid
  9. customThe precipitate was dried off
  10. washwashed with water
  11. customdried

출처 및 근거

ORD 기록
ord-50373ec866454dbc90f23bbbd0786341
출처 데이터셋
uspto-grants-1981_12
특허 번호
US04306072

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