(2,2-Diethoxyethyl)dimethylamine → HCID 131711015、化合物

HRID 1833420ノート

反応式

HRID 1833420 の反応式
[CH2:1]([O:3][CH:4]([O:9][CH2:10][CH3:11])[CH2:5][N:6]([CH3:8])[CH3:7])[CH3:2].[N+:12]([C:15]1[CH:20]=[CH:19][C:18]([C:21]2[O:25][C:24]([C:26]([CH2:28][Cl:29])=[O:27])=[CH:23][CH:22]=2)=[CH:17][CH:16]=1)([O-:14])=[O:13]>C(O)C>[OH2:3].[Cl-:29].[CH2:10]([O:9][CH:4]([O:3][CH2:1][CH3:2])[CH2:5][N+:6]([CH3:7])([CH3:8])[CH2:28][C:26]([C:24]1[O:25][C:21]([C:18]2[CH:19]=[CH:20][C:15]([N+:12]([O-:14])=[O:13])=[CH:16][CH:17]=2)=[CH:22][CH:23]=1)=[O:27])[CH3:11].[CH2:10]([O:9][CH:4]([O:3][CH2:1][CH3:2])[CH2:5][N+:6]([CH2:28][C:26]([C:24]1[O:25][C:21]([C:18]2[CH:19]=[CH:20][C:15]([N+:12]([O-:14])=[O:13])=[CH:16][CH:17]=2)=[CH:22][CH:23]=1)=[O:27])([CH3:7])[CH3:8])[CH3:11].[Cl-:29]

参加物

4

反応物 2

HCID 77163(2,2-Diethoxyethyl)dimethylamineHCID 213893612-Chloro-1-[5-(4-nitrophenyl)furan-2-yl]ethan-1-one

生成物 1

HCID 131711015HCID 131711015、化合物収率 86%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

Dimethylaminoacetaldehyde diethyl acetal (29 g, 0.18 mole) was added dropwise to a stirred mixture of 40 g (0.15 mole) of chloromethyl 5-(4-nitrophenyl)-2-furyl ketone in 750 ml of absolute ethanol at 30° over 15 minutes. The mixture was heated under reflux for 22 hrs and was filtered hot to remove a black insoluble material. The filtrate was cooled in ice, and the brown solid was filtered and discarded. The filtrate was diluted with 1.5 liters of anhydrous ether, and the solid which was deposited was collected by filtration to give 45 g (69%) of (2,2-diethoxyethyl)dimethyl[5-(4-nitrophenyl)-2-furoylmethyl] ammonium chloride hemihydrate. Two recrystallizations from CH3CN gave an analytical sample, m.p. 113°-118°.

後処理

  1. temperatureThe mixture was heated
  2. temperatureunder reflux for 22 hrs
  3. filtrationwas filtered hot
  4. customto remove a black insoluble material
  5. temperatureThe filtrate was cooled in ice
  6. filtrationthe brown solid was filtered
  7. additionThe filtrate was diluted with 1.5 liters of anhydrous ether
  8. filtrationthe solid which was deposited was collected by filtration

出典と根拠

ORDレコード
ord-3f0a2f3dd4d74a18ab0a46df57df333f
出典データセット
uspto-grants-1978_01
特許番号
US04066671

反応ノート

読み込み中…