Tetrahydrothiopyran-4-one → 3,4-dihydro-6-(1,1-dimethylethyl)-8-iodospiro-[2H-1,3-benzoxazine-2,4'-tetrahydrothiopyran]

HRID 372830

反応式

HRID 372830 の反応式
[NH2:1][CH2:2][C:3]1[CH:8]=[C:7]([C:9]([CH3:12])([CH3:11])[CH3:10])[CH:6]=[C:5]([I:13])[C:4]=1[OH:14].[S:15]1[CH2:20][CH2:19][C:18](=O)[CH2:17][CH2:16]1>C1C=CC=CC=1>[CH3:12][C:9]([C:7]1[CH:6]=[C:5]([I:13])[C:4]2[O:14][C:18]3([CH2:19][CH2:20][S:15][CH2:16][CH2:17]3)[NH:1][CH2:2][C:3]=2[CH:8]=1)([CH3:11])[CH3:10]

参加物

4

反応物 2

HCID 66173Tetrahydrothiopyran-4-oneHCID 1192862-Aminomethyl-4-t-butyl-6-iodophenol

生成物 1

HCID 128578993,4-dihydro-6-(1,1-dimethylethyl)-8-iodospiro-[2H-1,3-benzoxazine-2,4'-tetrahydrothiopyran]収率 62%

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

A mixture of 2-aminomethyl-4-(1,1-dimethylethyl)-6-iodophenol (3.0 g., 0.01 mole), tetrahydrothiopyran-4-one (1.18 g., 0.01 mole), and benzene (100 ml.), is refluxed under a Dean-Stark trap for 4 hr. The solvent is evaporated, and the residue is crystallized from ethanol to obtain 3,4-dihydro-6-(1,1-dimethylethyl)-8-iodospiro-[2H-1,3-benzoxazine-2,4'-tetrahydrothiopyran], (2.5 g.), m.p. 123°-124° C.

後処理

  1. temperatureis refluxed under a Dean-Stark trap for 4 hr
  2. customThe solvent is evaporated
  3. customthe residue is crystallized from ethanol

出典と根拠

ORDレコード
ord-3ecb22d8e9f54b36971f396c14b4a2c7
出典データセット
uspto-grants-1978_05
特許番号
US04092414

関連ノート

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