Dichloromethane methanol → HCID 178516473、化合物

HRID 2178985ノート

反応式

HRID 2178985 の反応式
[S:1]1[C:5]([NH:6][CH:7]=[C:8]2[C:13](=[O:14])OC(C)(C)OC2=O)=[CH:4][C:3]2[CH2:18][CH2:19][CH2:20][C:2]1=2.ClCCl.CO>O(C1C=CC=CC=1)C1C=CC=CC=1>[C:4]12[C:13]([OH:14])=[CH:8][CH:7]=[N:6][C:5]=1[S:1][C:2]1[CH2:20][CH2:19][CH2:18][C:3]2=1

参加物

4

反応物 2

HCID 21226129Dichloromethane methanolHCID 867080805-[([4H,5H,6H-cyclopenta[b]thiophen-2-yl]amino)methylidene]-2,2-dimethyl-1,3-dioxane-4,6-dione

生成物 1

HCID 178516473HCID 178516473、化合物収率 80%

試薬・触媒・溶媒 1

HCID 7583Diphenyl Ether溶媒

実験手順

A solution of 5-[([4H,5H,6H-cyclopenta[b]thiophen-2-yl]amino)methylidene]-2,2-dimethyl-1,3-dioxane-4,6-dione (540 mg, 1.84 mmol, 1.00 equiv) in phenoxybenzene (5 mL) was heated at 220° C. for 30 min under nitrogen. After cooling to room temperature, the residue was applied onto a silica gel column with dichloromethane/methanol (10:1) to give the desired 7-thia-9-azatricyclo[6.4.0.0^[2,6]]dodeca-1(8),2(6),9,11-tetraen-12-ol (0.28 g, 80%) as a brown solid. MS (ES): m/z 192 (M+H)+.

出典と根拠

ORDレコード
ord-5d3ae8ed2b5b45dc9dcdb05b460367a1
出典データセット
uspto-grants-2015_06
特許番号
US09067948B2

反応ノート

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