Acetic Anhydride → 6-(2-Ethylaminophenyl)-5,6,7,8-tetrahydronaphthalen-2-ol

HRID 1950115ノート

反応式

HRID 1950115 の反応式
COC1C=C2C(=CC=1)CC(C1C=CC=CC=1N)CC2.C(OC(=O)C)(=O)C.[OH:27][C:28]1[CH:29]=[C:30]2[C:35](=[CH:36][CH:37]=1)[CH2:34][CH:33]([C:38]1[CH:43]=[CH:42][CH:41]=[CH:40][C:39]=1[NH:44][C:45](=O)[CH3:46])[CH2:32][CH2:31]2>N1C=CC=CC=1>[CH2:45]([NH:44][C:39]1[CH:40]=[CH:41][CH:42]=[CH:43][C:38]=1[CH:33]1[CH2:32][CH2:31][C:30]2[CH:29]=[C:28]([OH:27])[CH:37]=[CH:36][C:35]=2[CH2:34]1)[CH3:46]

参加物

5

反応物 3

HCID 7918Acetic AnhydrideHCID 230875022-(6-Methoxy-1,2,3,4-tetrahydronaphthalen-2-yl)phenylamineHCID 66626221N-[2-(6-hydroxy-1,2,3,4-tetrahydronaphthalen-2-yl)phenyl]acetamide

生成物 1

HCID 230874696-(2-Ethylaminophenyl)-5,6,7,8-tetrahydronaphthalen-2-ol

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

A mixture of 2-(6-methoxy-1,2,3,4-tetrahydronaphthalen-2-yl)phenylamine (3.7 g), acetic anhydride (19 ml) and pyridine (19 ml) was stirred for 1 hour at room temperature. The reaction solution was concentrated in vacuo, then ethyl acetate (20 ml) and chloroform (5 ml) were added thereto, the crystal that was precipitated was filtered and dried. Synthesized from the total amount of the resulting N-[2-(6-methoxy-1,2,3,4-tetrahydronaphthalen-2-yl)phenyl]acetamide according to an analogous synthetic method to Example 364 described below, the total amount of N-[2-(6-hydroxy-1,2,3,4-tetrahydronaphthalen-2-yl)phenyl]acetamide was used according to an analogous synthetic method to Example 337 described below to provide the title compound (2.3 g).

後処理

  1. concentrationThe reaction solution was concentrated in vacuo
  2. additionethyl acetate (20 ml) and chloroform (5 ml) were added
  3. customthe crystal that was precipitated
  4. filtrationwas filtered
  5. customdried
  6. customSynthesized from the total amount of the resulting N-[2-(6-methoxy-1,2,3,4-tetrahydronaphthalen-2-yl)phenyl]acetamide according to an analogous synthetic method to Example 364

出典と根拠

ORDレコード
ord-e73bf81b3c2a426b96c99c6577093465
出典データセット
uspto-grants-2013_03
特許番号
US08399520B2

反応ノート

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