Water → HCID 13519498, 화합물

HRID 280142

반응식

HRID 280142 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

HCID 13519498HCID 13519498, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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.)

후처리

  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

출처 및 근거

ORD 기록
ord-64b00036f00c41938961949f3d284e48
출처 데이터셋
uspto-grants-1986_05
특허 번호
US04588719

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