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Benzil-di(beta-bromoethyl)ketal → Benzil-di(beta-phthalimidoethyl)ketal

HRID 1633335
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인쇄 미리보기

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HRID 1633335 반응식
Br[CH2:2][CH2:3][O:4][C:5]([O:20][CH2:21][CH2:22]Br)([C:12]([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)=[O:13])[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1.[C:24]1(=[O:34])[NH:28][C:27](=[O:29])[C:26]2=[CH:30][CH:31]=[CH:32][CH:33]=[C:25]12.[K]>CN(C=O)C>[C:24]1(=[O:34])[N:28]([CH2:2][CH2:3][O:4][C:5]([O:20][CH2:21][CH2:22][N:28]2[C:27](=[O:29])[C:26]3=[CH:30][CH:31]=[CH:32][CH:33]=[C:25]3[C:24]2=[O:34])([C:12]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)=[O:13])[C:6]2[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=2)[C:27](=[O:29])[C:26]2=[CH:30][CH:31]=[CH:32][CH:33]=[C:25]12
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 2326685Benzil-di(beta-bromoethyl)ketalHCID 24194345Phthalimide potassium salt

생성물 1

HCID 20440909Benzil-di(beta-phthalimidoethyl)ketal수율 96.4%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

Benzil-di(β-bromoethyl)ketal (8.84 g) and 7.4 g of potassium phthalimide were dissolved in 50 ml of DMF, and reacted at 50° to 60° C. for 6 hours. When the reaction mixture was poured into 100 ml of ice water, white crystals formed. The crystals were collected by filtration, well washed with water, and dried to give 11 g of benzil-di-(β-phthalimidoethyl)ketal in a yield of 96%. Recrystallization from a mixture of ethanol and chloroform afforded crystals having a melting point of 132° to 134° C. The product is referred to as initiator 2.

후처리

  1. customreacted at 50° to 60° C. for 6 hours
  2. customformed
  3. filtrationThe crystals were collected by filtration
  4. washwell washed with water
  5. customdried

출처 및 근거

ORD 기록
ord-93607d8e842d4cf1960d29e090b809ca
출처 데이터셋
uspto-grants-1984_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04480094

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