HCID 58065823、化合物 → HCID 71253947、化合物

HRID 1028314ノート

反応式

HRID 1028314 の反応式
[CH3:1][Mg]Br.[Br:4][C:5]1[CH:6]=[CH:7][C:8]2[N:9]([CH2:19][C:20](=[O:29])[CH2:21][O:22][C:23]3[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=3)[C:10]3[C:15]([C:16]=2[CH:17]=1)=[CH:14][C:13]([Br:18])=[CH:12][CH:11]=3>C1COCC1>[Br:4][C:5]1[CH:6]=[CH:7][C:8]2[N:9]([CH2:19][C:20]([CH3:1])([OH:29])[CH2:21][O:22][C:23]3[CH:24]=[CH:25][CH:26]=[CH:27][CH:28]=3)[C:10]3[C:15]([C:16]=2[CH:17]=1)=[CH:14][C:13]([Br:18])=[CH:12][CH:11]=3

参加物

4

反応物 2

HCID 58065823HCID 58065823、化合物HCID 178418573HCID 178418573、化合物

生成物 1

HCID 71253947HCID 71253947、化合物収率 89%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

Methylmagnesium bromide (92 μl, 3.0 M in THF) was added to an ice-cooled solution of title compound of example 103, step 1, 1-(3,6-dibromo-9H-carbazol-9-yl)-3-phenoxypropan-2-one (86 mg, 0.18 mmol) in anhydrous THF (1.8 ml). The reaction was stirred in the gently warming ice bath for 6 hours, and then quenched by addition of water. The crude mixture was diluted with EtOAc and washed with saturated sodium bicarbonate, water and then brine. The organic layer was dried over Na2SO4, filtered and condensed. Some unreacted starting material was precipitated from ˜50% acetone/hexanes. The condensed filtrate was carried forward. Yield=89%. MS (ESI), m/z: calculated 486.98. found 531.7 (M+HCOO−).

出典と根拠

ORDレコード
ord-021ddd86244c404186117e2ea045e6a4
出典データセット
uspto-grants-2014_05
特許番号
US08735440B2

反応ノート

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