1-Chloromethyl-2-methylnaphthalene → HCID 68571179、化合物

HRID 18777ノート

反応式

HRID 18777 の反応式
[C:1]1([C@H:7]2[C@@H:11]([C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=3)[NH:10][C:9](=[S:18])[NH:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[Cl:19][CH2:20][C:21]1[C:30]2[C:25](=[CH:26][CH:27]=[CH:28][CH:29]=2)[CH:24]=[CH:23][C:22]=1[CH3:31]>CCO>[ClH:19].[CH3:31][C:22]1[CH:23]=[CH:24][C:25]2[C:30](=[CH:29][CH:28]=[CH:27][CH:26]=2)[C:21]=1[CH2:20][S:18][C:9]1[NH:8][C@H:7]([C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)[C@H:11]([C:12]2[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=2)[N:10]=1

参加物

4

反応物 2

HCID 811061-Chloromethyl-2-methylnaphthaleneHCID 45258634cis-4,5-Diphenylimidazolidine-2-thione

生成物 1

HCID 68571179HCID 68571179、化合物収率 65.5%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of intermediate 25 (200 mg, 0.786 mmol) and 1-chloromethyl-2-methyl-naphthalene (299 mg, 1.57 mmol) in abs. EtOH (2 mL) is heated at 95° C. for 24 h. The reaction mixture is cooled to RT, evaporated to dryness, and the residue suspended in Et2O. The insoluble material is filtered to give 229 mg of the product 226. 1H NMR (DMSO-d6) δ 11.40 (s, 2 H), 8.36 (d, 1 H), 8.10-7.80 (m, 2 H), 7.80-7.30 (m, 3 H), 7.30-6.75 (m, 10 H), 5.90 (s, 2 H), 5.30 (s, 2 H), 2.62 (s, 3 H); MS: m/z 409 (M++1).

後処理

  1. customevaporated to dryness
  2. filtrationThe insoluble material is filtered

出典と根拠

ORDレコード
ord-649d97d8f8864912961228516f84466d
出典データセット
uspto-grants-2010_06
特許番号
US07741493B2

反応ノート

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