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Benzyl Chloride → (cis)-2-Benzyl-4-(3,4-dimethoxyphenyl)-4a,5,6,7,8,8a-hexahydro-2H-phthalazin-1-one

HRID 1871402
ノート
印刷プレビュー

反応式

HRID 1871402 の反応式
[H-].[Na+].[CH3:3][O:4][C:5]1[CH:6]=[C:7]([C:13]2[C@H:22]3[C@H:17]([CH2:18][CH2:19][CH2:20][CH2:21]3)[C:16](=[O:23])[NH:15][N:14]=2)[CH:8]=[CH:9][C:10]=1[O:11][CH3:12].[CH2:24](Cl)[C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1>CN(C)C=O>[CH2:24]([N:15]1[N:14]=[C:13]([C:7]2[CH:8]=[CH:9][C:10]([O:11][CH3:12])=[C:5]([O:4][CH3:3])[CH:6]=2)[C@H:22]2[C@H:17]([CH2:18][CH2:19][CH2:20][CH2:21]2)[C:16]1=[O:23])[C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 7503Benzyl ChlorideHCID 24758Sodium hydrideHCID 10913208(cis)-4-(3,4-Dimethoxyphenyl)-4a,5,6,7,8,8a-hexahydro-2H-phthalazin-1-one

生成物 1

HCID 70001660(cis)-2-Benzyl-4-(3,4-dimethoxyphenyl)-4a,5,6,7,8,8a-hexahydro-2H-phthalazin-1-one

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

6 mmol of a 60% suspension of sodium hydride in mineral oil was added to a suspension of 5 mmol of compound 1 in about 40 ml of dimethylformamide, under a flow of nitrogen at room temperature. After stirring this mixture for 30 minutes, 7 mmol of benzylchloride was added and the resulting mixture was stirred for another 4 hours, after which the solvent was evaporated. The residue was partitioned between ethyl acetate and water, the organic layer was dried over magnesium sulfate and evaporated. The residue was crystallized from methanol. M.p. 117°-118° C.

後処理

  1. stirringthe resulting mixture was stirred for another 4 hours
  2. customafter which the solvent was evaporated
  3. customThe residue was partitioned between ethyl acetate and water
  4. dry with materialthe organic layer was dried over magnesium sulfate
  5. customevaporated
  6. customThe residue was crystallized from methanol

出典と根拠

ORDレコード
ord-88fcb6379b564b49991aee24f693ab72
出典データセット
uspto-grants-2000_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06103718

反応ノート

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