Water → 1-(Tert-butyldiphenylsilyloxymethyl)-2,6-dimethyl-3-(phthalimidoacetylamino)benzene

HRID 636492ノート

反応式

HRID 636492 の反応式
[NH2:1][C:2]1[C:3]([CH3:28])=[C:4]([CH2:9][O:10][Si:11]([C:24]([CH3:27])([CH3:26])[CH3:25])([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[C:5]([CH3:8])=[CH:6][CH:7]=1.[C:29]1(=[O:43])[N:33]([CH2:34][C:35](Cl)=[O:36])[C:32](=[O:38])[C:31]2=[CH:39][CH:40]=[CH:41][CH:42]=[C:30]12.O>N1C=CC=CC=1.CN(C)C=O>[Si:11]([O:10][CH2:9][C:4]1[C:5]([CH3:8])=[CH:6][CH:7]=[C:2]([NH:1][C:35](=[O:36])[CH2:34][N:33]2[C:32](=[O:38])[C:31]3=[CH:39][CH:40]=[CH:41][CH:42]=[C:30]3[C:29]2=[O:43])[C:3]=1[CH3:28])([C:24]([CH3:25])([CH3:27])[CH3:26])([C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1)[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1

参加物

6

反応物 3

HCID 962WaterHCID 812422H-Isoindole-2-acetyl chloride, 1,3-dihydro-1,3-dioxo-HCID 107391063-Amino-1-(tert-butyldiphenylsilyloxymethyl)-2,6-dimethylbenzene

生成物 1

HCID 105074021-(Tert-butyldiphenylsilyloxymethyl)-2,6-dimethyl-3-(phthalimidoacetylamino)benzene収率 94.2%

試薬・触媒・溶媒 2

HCID 1049Pyridine溶媒HCID 6228Dimethylformamide溶媒

実験手順

To a suspension of 3-amino-1-(tert-butyldiphenylsilyloxymethyl)-2,6-dimethylbenzene (42.4 g) in pyridine (17.2 g) and dimethylformamide (212 ml) was dropwise added phthalimidoacetyl chloride (25.6 g) over the period of 15 minutes under ice-cooling, and the mixture was stirred for 1 hour at the same temperature. To the reaction mixture was added water, and the resulting precipitates were collected by filtration and washed with acetonitrile to give 1-(tert-butyldiphenylsilyloxymethyl)-2,6-dimethyl-3-(phthalimidoacetylamino)benzene (59.1 g) as colorless crystals.

後処理

  1. customover the period of 15 minutes
  2. temperaturecooling
  3. customthe resulting precipitates
  4. filtrationwere collected by filtration
  5. washwashed with acetonitrile

出典と根拠

ORDレコード
ord-75f73dd2c7e74aa9bea5384e06a66f71
出典データセット
uspto-grants-2001_02
特許番号
US06194396B1

反応ノート

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