Methanol → 4-(2,2,4,4-Tetramethyl-8-prop-2-ynyl-chroman-6-ylethynyl)-phenyl-acetic acid

HRID 898679ノート

反応式

HRID 898679 の反応式
C[O:2][C:3](=[O:34])[CH2:4][C:5]1[CH:10]=[CH:9][C:8]([C:11]#[C:12][C:13]2[CH:14]=[C:15]3[C:20](=[C:21]([CH2:23][C:24]#[C:25][Si](C)(C)C)[CH:22]=2)[O:19][C:18]([CH3:31])([CH3:30])[CH2:17][C:16]3([CH3:33])[CH3:32])=[CH:7][CH:6]=1.CO.O1CCCC1.O.[OH-].[Li+]>O>[CH3:30][C:18]1([CH3:31])[CH2:17][C:16]([CH3:32])([CH3:33])[C:15]2[C:20](=[C:21]([CH2:23][C:24]#[CH:25])[CH:22]=[C:13]([C:12]#[C:11][C:8]3[CH:7]=[CH:6][C:5]([CH2:4][C:3]([OH:34])=[O:2])=[CH:10][CH:9]=3)[CH:14]=2)[O:19]1

参加物

6

反応物 4

HCID 887MethanolHCID 8028TetrahydrofuranHCID 168937Lithium hydroxide, monohydrateHCID 69216503HCID 69216503、化合物2 回

生成物 1

HCID 102873324-(2,2,4,4-Tetramethyl-8-prop-2-ynyl-chroman-6-ylethynyl)-phenyl-acetic acid

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Following general procedure K and using {4-[2,2,4,4-tetramethyl-8-(3-trimethylsilanyl-prop-2-ynyl)-chroman-6-ylethynyl]-phenyl}-acetic acid methyl ester (Compound 48, 0.105 g, 0.21 mmol), methanol (3 mL), tetrahydrofuran (3 mL), water (1.5 mL) and lithium hydroxide monohydrate (0.128 g, 3.07 mmol), the title compound was obtained as a pale yellow solid (0.077 g, 95%). 1H NMR (300 MHz, CDCl3): δ7.51 (d, 1H, J=2.2 Hz), 7.49 (d, 2H, J=8.2 Hz), 7.39 (d, 1H, J=2.2 Hz), 7.25 (d, 2H, J=8.2 Hz), 3.66 (s, 2H), 3.52 (d, 2H, J=2.6 Hz), 2.61 (t, 1H, J=2.6 Hz), 1.83 (s, 2H), 1.36 (s, 6H), 1.35 (s, 6H).

出典と根拠

ORDレコード
ord-7b89d6a853594c888727bbbb854db39b
出典データセット
uspto-grants-2008_04
特許番号
US07351737B2

反応ノート

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