Potassium Hydroxide → 1(3H)-Isobenzofuranone, 3-[2,4-bis(dimethylamino)phenyl]-6-(dimethylamino)-3-[4-(dimethylamino)phenyl]-

HRID 569673노트

반응식

HRID 569673 반응식
[CH3:1][N:2]([CH3:34])[C:3]1[CH:30]=[C:29]([N:31]([CH3:33])[CH3:32])[CH:28]=[CH:27][C:4]=1[CH:5]([C:15]1[CH:23]=[CH:22][C:21]([N:24]([CH3:26])[CH3:25])=[CH:20][C:16]=1[C:17]([OH:19])=[O:18])[C:6]1[CH:11]=[CH:10][C:9]([N:12]([CH3:14])[CH3:13])=[CH:8][CH:7]=1.[OH-].[K+].C(=O)(O)[O-].[Na+]>O>[CH3:34][N:2]([CH3:1])[C:3]1[CH:30]=[C:29]([N:31]([CH3:33])[CH3:32])[CH:28]=[CH:27][C:4]=1[C:5]1([C:6]2[CH:7]=[CH:8][C:9]([N:12]([CH3:13])[CH3:14])=[CH:10][CH:11]=2)[C:15]2[C:16](=[CH:20][C:21]([N:24]([CH3:25])[CH3:26])=[CH:22][CH:23]=2)[C:17](=[O:19])[O:18]1

참가 물질

5

반응물 3

HCID 14797Potassium HydroxideHCID 112438HCID 112438, 화합물HCID 516892Sodium Bicarbonate

생성물 1

HCID 1036931(3H)-Isobenzofuranone, 3-[2,4-bis(dimethylamino)phenyl]-6-(dimethylamino)-3-[4-(dimethylamino)phenyl]-수율 79.6%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A solution of 29.78 g of 2-[2,4,4'-tris(dimethylamino)benzhydryl]-5-dimethylaminobenzoic acid prepared as described in part B above, 450.0 g of water and 16.2 g of flake potassium hydroxide was prepared and the pH adjusted to 10.0 by the gradual addition of sodium bicarbonate. The solution was then heated at approximately 75° C. under an atmosphere of oxygen at 60-65 psi for approximately six hours in an agitated stainless steel autoclave. The solid which separated was collected by filtration at ambient temperature, washed with water until alkali free when tested with Brilliant Yellow test paper and dried. The dried solid was slurried with hexane at room temperature, filtered and dried to obtain 23.6 g of 3-(2,4-bis[dimethylamino]phenyl)-3-(4-dimethylaminophenyl)-6-dimethylaminophthalide (Formula I: R=CH3 ; X=H; Y=4-(CH3)2NC6H4 ; Z=2,4-[(CH3)2N]2C6H3) a pale blue-colored solid melting at 171°-172° C.

후처리

  1. customwas prepared
  2. customThe solid which separated
  3. filtrationwas collected by filtration at ambient temperature
  4. washwashed with water until alkali free when
  5. customdried
  6. customwas slurried with hexane at room temperature
  7. filtrationfiltered
  8. customdried

출처 및 근거

ORD 기록
ord-3139c3b61c624859a062e533a1578b93
출처 데이터셋
uspto-grants-1988_03
특허 번호
US04732991

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