Hydrochloric Acid → Methyl 4-hydrazinyl-2-methoxybenzoate

HRID 59249

反応式

HRID 59249 の反応式
[NH2:1][C:2]1[CH:11]=[CH:10][C:5]([C:6]([O:8][CH3:9])=[O:7])=[C:4]([O:12][CH3:13])[CH:3]=1.[N:14]([O-])=O.[Na+].Cl>O>[NH:1]([C:2]1[CH:11]=[CH:10][C:5]([C:6]([O:8][CH3:9])=[O:7])=[C:4]([O:12][CH3:13])[CH:3]=1)[NH2:14]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 168705Methyl 4-amino-o-anisateHCID 23668193Sodium Nitrite

生成物 1

HCID 45089366Methyl 4-hydrazinyl-2-methoxybenzoate収率 108,113%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

The title compound was prepared according to the procedure described in step-2 of Intermediate-7 by using methyl 4-amino-2-methoxybenzoate (10.0 g, 0.055 mol), stannous chloride (31.00 g, 0.138 mmol), sodium nitrite (4.57 g, 0.066 mmol), 6 N HCl (200 mL) and water (100 mL) to afford 14.0 g of desired product. 1H NMR (300 MHz, DMSO d6): δ 3.73 (s, 3H), 3.80 (s, 3H), 6.51 (d, J=8.4 Hz, 1H), 6.69 (s, 1H), 7.68 (d, J=8.4 Hz, 1H), 8.75 (br s, 1H), 10.28 (br hump, 2H); MS (m/z): 197.01 (M+H)+.

後処理

  1. customThe title compound was prepared

出典と根拠

ORDレコード
ord-46f8d2f98c9945eb9e7783f9b2beb222
出典データセット
uspto-grants-2016_09
特許番号
US09439890B2

関連ノート

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