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Water → N-alpha-Phenylethylphenoxazine

HRID 247375
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HRID 247375 반응식
[CH:1]1[C:14]2[NH:13][C:12]3[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=3)[O:6][C:5]=2[CH:4]=[CH:3][CH:2]=1.[H-].[Na+].[C:17]1([CH:23](Cl)[CH3:24])[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1.O>CN(C)C=O>[C:17]1([CH:23]([N:13]2[C:14]3[CH:1]=[CH:2][CH:3]=[CH:4][C:5]=3[O:6][C:7]3[C:12]2=[CH:11][CH:10]=[CH:9][CH:8]=3)[CH3:24])[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 12648(1-Chloroethyl)benzeneHCID 24758Sodium hydrideHCID 67278Phenoxazine

생성물 1

HCID 14031257N-alpha-Phenylethylphenoxazine

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

A solution of phenoxazine 76 g, 0.417 mol (Aldrich Chemical Co., Milwaukee, WI, Cat. No. P1,585-8) in dry dimethylformamide (120 ml) was added to a stirred suspension of sodium hydride (22 g, 0.458 mol, 50% suspension in mineral oil) in dry dimethylformamide (500 ml). After 1 hour at room temperature α-phenylethyl chloride (59 g, 0.43 mol) was added dropwise and when the addition was completed, stirring was continued for another 30 min. The solution was poured into water, the product extracted with ethyl acetate, the extract washed with water, and dried over sodium sulfate. The solvent was removed under reduced pressure. N-α-Phenylethylphenoxazine was crystallized from ether-hexane, mp 100° C.

후처리

  1. additionwhen the addition
  2. extractionthe product extracted with ethyl acetate
  3. washthe extract washed with water
  4. dry with materialdried over sodium sulfate
  5. customThe solvent was removed under reduced pressure
  6. customN-α-Phenylethylphenoxazine was crystallized from ether-hexane, mp 100° C.

출처 및 근거

ORD 기록
ord-f3b6d518f76f4e13a3e66dde83eec807
출처 데이터셋
uspto-grants-1987_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04707473

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