Acetic Anhydride → HCID 20523567、化合物

HRID 1413880ノート

反応式

HRID 1413880 の反応式
[CH2:1]([N:5]1[C:13]2[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=2)[C:7]([C:14]([C:16]2[CH:24]=[CH:23][CH:22]=[CH:21][C:17]=2[C:18](O)=[O:19])=[O:15])=[C:6]1[CH3:25])[CH2:2][CH2:3][CH3:4].[CH3:26][N:27]([CH3:37])[C:28]1[CH:33]=[CH:32][CH:31]=[C:30]([N:34]([CH3:36])[CH3:35])[CH:29]=1.C(OC(=O)C)(=O)C.[OH-].[Na+]>O>[CH3:35][N:34]([CH3:36])[C:30]1[CH:29]=[C:28]([N:27]([CH3:37])[CH3:26])[CH:33]=[CH:32][C:31]=1[C:14]1([C:7]2[C:8]3[C:13](=[CH:12][CH:11]=[CH:10][CH:9]=3)[N:5]([CH2:1][CH2:2][CH2:3][CH3:4])[C:6]=2[CH3:25])[C:16]2[C:17](=[CH:21][CH:22]=[CH:23][CH:24]=2)[C:18](=[O:19])[O:15]1

参加物

6

反応物 4

HCID 7918Acetic AnhydrideHCID 14798Sodium HydroxideHCID 897151,3-Benzenediamine, N1,N1,N3,N3-tetramethyl-HCID 105559Benzoic acid, 2-[(1-butyl-2-methyl-1H-indol-3-yl)carbonyl]-

生成物 1

HCID 20523567HCID 20523567、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of 3.35 g (0.01 mole) of 2-[(1-n-butyl-2-methyl-3-indolyl)carbonyl]benzoic acid, prepared as described in part A above, 1.80 g (0.011 mole) of N,N,N',N'-tetramethyl-m-phenylenediamine and five ml of acetic anhydride was stirred at ambient temperature for a period of approximately 18 hours. The reaction mixture was then poured into a mixture of 40 ml of water, 40 ml of ligroin and 20 ml of 10 percent aqueous sodium hydroxide. The ligroin layer was separated and the white crystals which separated from the solution on standing, were collected by filtration and dried to obtain 3-[2,4-bis(dimethylamino)phenyl]-3-(1-n-butyl-2-methyl-3-indolyl)phthalide (Formula III: R0 =R1 =R2 =R3 =Y1 =H; R=R5 =CH3 ; R4 =N(CH3)2 ; R6 =(CH2)3CH3) which melted at 165°-167° C. A characteristic infrared maximum appeared at 1752 cm-1 (C=O; s). A toluene solution of the product spotted on silica gel developed an intense purple-colored image.

後処理

  1. customprepared
  2. customThe ligroin layer was separated
  3. customthe white crystals which separated from the solution on standing
  4. filtrationwere collected by filtration
  5. customdried

出典と根拠

ORDレコード
ord-8f8edc45c9344a1baa8bb3ebb049f833
出典データセット
uspto-grants-1981_02
特許番号
US04251446

反応ノート

読み込み中…