Water → HCID 13519498、化合物

HRID 280142ノート

反応式

HRID 280142 の反応式
[OH:1][C:2]1[CH:11]=[C:10]2[C:5]([CH2:6][CH2:7][CH2:8][C:9]2=[O:12])=[CH:4][CH:3]=1.C[O-].[Na+].Br[CH2:17][CH2:18][CH2:19][N:20]1[C:24](=[O:25])[C:23]2=[CH:26][CH:27]=[CH:28][CH:29]=[C:22]2[C:21]1=[O:30].O>CN(C)C=O>[C:21]1(=[O:30])[N:20]([CH2:19][CH2:18][CH2:17][O:1][C:2]2[CH:11]=[C:10]3[C:5]([CH2:6][CH2:7][CH2:8][C:9]3=[O:12])=[CH:4][CH:3]=2)[C:24](=[O:25])[C:23]2=[CH:26][CH:27]=[CH:28][CH:29]=[C:22]12

参加物

6

反応物 4

HCID 962WaterHCID 21611N-3-BromopropylphthalimideHCID 5718187-hydroxy-3,4-dihydro-2H-naphthalen-1-oneHCID 10942334Sodium Methoxide

生成物 1

HCID 13519498HCID 13519498、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

7-Hydroxy-1-tetralone (33.3 g) is dissolved in dimethylformamide (325 ml) and the mixture is cooled in an ice bath. Sodium methoxide (11.07 g) is added to the mixture. After the mixture is stirred for 3 min., N-(3-bromopropyl)phthalimide (54.96 g) is added to the mixture; stirring is continued and the reaction mixture stirred overnight. The resulting mixture is poured into H2O (650 ml), stirred for 1 hour, filtered, washed with H2O and air dried. The resulting fluffy near-white solid (62.8 g) is crystallized from ethyl acetate to give the desired product, a fluffy white solid (M.P. 149°-150° C.)

後処理

  1. temperaturethe mixture is cooled in an ice bath
  2. stirringstirring
  3. stirringthe reaction mixture stirred overnight
  4. stirringstirred for 1 hour
  5. filtrationfiltered
  6. washwashed with H2O and air
  7. customdried
  8. customThe resulting fluffy near-white solid (62.8 g) is crystallized from ethyl acetate

出典と根拠

ORDレコード
ord-64b00036f00c41938961949f3d284e48
出典データセット
uspto-grants-1986_05
特許番号
US04588719

反応ノート

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