4-chlorobenzyl Isothiocyanate → 1-(4-Chlorobenzyl)-3-(6-methoxy-1,2,3,4-tetrahydronaphthalen-1-yl)thiourea

HRID 656307ノート

反応式

HRID 656307 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][CH:12]=1)[CH:9]([NH2:13])[CH2:8][CH2:7][CH2:6]2.[Cl:14][C:15]1[CH:24]=[CH:23][C:18]([CH2:19][N:20]=[C:21]=[S:22])=[CH:17][CH:16]=1>C(OCC)(=O)C>[Cl:14][C:15]1[CH:16]=[CH:17][C:18]([CH2:19][NH:20][C:21]([NH:13][CH:9]2[C:10]3[C:5](=[CH:4][C:3]([O:2][CH3:1])=[CH:12][CH:11]=3)[CH2:6][CH2:7][CH2:8]2)=[S:22])=[CH:23][CH:24]=1

参加物

4

反応物 2

HCID 194084-chlorobenzyl IsothiocyanateHCID 382506-Methoxy-1,2,3,4-tetrahydro-1-naphthalenylamine

生成物 1

HCID 590880671-(4-Chlorobenzyl)-3-(6-methoxy-1,2,3,4-tetrahydronaphthalen-1-yl)thiourea収率 99%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒2 回

実験手順

The compound 32-1 (100 mg) prepared according to the same procedure as described in Step 1 was dissolved in ethyl acetate (4 ml) and to the solution were added a solution of 4-chlorobenzylisothiocyanate (123 mg) in ethyl acetate (2 ml), followed by stirring at room temperarure for 18 hours. The obtained reaction mixture was concentrated under reduced pressure and purified by column-chromatography (hexane/ethyl acetate=2/1) to yield the compound 32-2 (201 mg, 99%).

後処理

  1. customThe obtained reaction mixture
  2. concentrationwas concentrated under reduced pressure
  3. custompurified by column-chromatography (hexane/ethyl acetate=2/1)

出典と根拠

ORDレコード
ord-5d61cce8bcdf431994f564b5fbbc3459
出典データセット
uspto-grants-2011_12
特許番号
US08071650B2

反応ノート

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