Phthalimide → 5-(4-Nitrophenyl)-8-(phthalimidomethyl)-9H-1,3-dioxolo[4,5-h][2,3]-benzodiazepine

HRID 1359572

반응식

HRID 1359572 반응식
N(C(OCC)=O)=NC(OCC)=O.O[CH2:14][C:15]1[CH2:21][C:20]2[CH:22]=[C:23]3[O:28][CH2:27][O:26][C:24]3=[CH:25][C:19]=2[C:18]([C:29]2[CH:34]=[CH:33][C:32]([N+:35]([O-:37])=[O:36])=[CH:31][CH:30]=2)=[N:17][N:16]=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[C:57]1(=[O:67])[NH:61][C:60](=[O:62])[C:59]2=[CH:63][CH:64]=[CH:65][CH:66]=[C:58]12>C1COCC1>[N+:35]([C:32]1[CH:33]=[CH:34][C:29]([C:18]2[C:19]3[CH:25]=[C:24]4[O:26][CH2:27][O:28][C:23]4=[CH:22][C:20]=3[CH2:21][C:15]([CH2:14][N:61]3[C:60](=[O:62])[C:59]4=[CH:63][CH:64]=[CH:65][CH:66]=[C:58]4[C:57]3=[O:67])=[N:16][N:17]=2)=[CH:30][CH:31]=1)([O-:37])=[O:36]

참가 물질

6

반응물 4

HCID 6809PhthalimideHCID 11776TriphenylphosphineHCID 220568ethyl N-ethoxycarbonyliminocarbamateHCID 181831918-Hydroxymethyl-5-(4-nitrophenyl)-9H-1,3-dioxolo[4,5-h][2,3]benzodiazepine2회

생성물 1

HCID 181831245-(4-Nitrophenyl)-8-(phthalimidomethyl)-9H-1,3-dioxolo[4,5-h][2,3]-benzodiazepine

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

A solution of 1.25 ml (8.05 mmol) of diethyl azodicarboxylate in 7 ml of THF is added in drops to a stirred solution of 2.60 g (7.66 mmol) of 8-hydroxymethyl-5-(4-nitrophenyl)-9H-1,3-dioxolo[4,5-h][2,3]-benzodiazepine (starting compound III.), 2.11 g (8.05 mmol) of triphenylphosphine and 1.18 g (8.05 mmol) of phthalimide in 130 ml of dry THF at room temperature. The mixture is stirred for 24 hours at this temperature. Then, the precipitated product is suctioned off and washed with ethanol. 2.87 g (80%) of the title compound, which can be further processed without further purification, is obtained.

후처리

  1. washwashed with ethanol
  2. custom2.87 g (80%) of the title compound, which can be further processed without further purification
  3. customis obtained

출처 및 근거

ORD 기록
ord-ccef06c579284bcdbc238ad1865a9f60
출처 데이터셋
uspto-grants-2003_07
특허 번호
US06600036B2

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