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

HRID 430656

反応式

HRID 430656 の反応式
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]

参加物

6

反応物 4

HCID 6809PhthalimideHCID 11776TriphenylphosphineHCID 220568ethyl N-ethoxycarbonyliminocarbamateHCID 181831918-Hydroxymethyl-5-(4-nitrophenyl)-9H-1,3-dioxolo[4,5-h][2,3]benzodiazepine2 回

生成物 1

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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-6429d3d3bc204717b1ac0026f57232c5
出典データセット
uspto-grants-2001_11
特許番号
US06323197B1

関連ノート

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