Hydrochloric Acid → 5-(2-(9H-fluoren-9-ylidene)acetamido)pentanoic acid

HRID 1926187ノート

反応式

HRID 1926187 の反応式
C[O:2][C:3](=[O:25])[CH2:4][CH2:5][CH2:6][CH2:7][NH:8][C:9](=[O:24])[CH:10]=[C:11]1[C:23]2[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=2[C:17]2[C:12]1=[CH:13][CH:14]=[CH:15][CH:16]=2.CO.[Li+].[OH-].Cl>O>[CH:13]1[C:12]2[C:11](=[CH:10][C:9]([NH:8][CH2:7][CH2:6][CH2:5][CH2:4][C:3]([OH:25])=[O:2])=[O:24])[C:23]3[C:18](=[CH:19][CH:20]=[CH:21][CH:22]=3)[C:17]=2[CH:16]=[CH:15][CH:14]=1

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 887MethanolHCID 3939Lithium HydroxideHCID 579720535-(2-(9H-fluoren-9-ylidene)acetamido)pentanoic acid methyl ester

生成物 1

HCID 579720655-(2-(9H-fluoren-9-ylidene)acetamido)pentanoic acid収率 87%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

5-(2-(9H-fluoren-9-ylidene)acetamido)pentanoic acid methyl ester (335 mg, 1 mmol) and 300 ml of CH3OH were stirred at room temperature while 25 ml of 4 N solution of LiOH in H2O was added. The mixture was stirred for 24 hours at room temperature. The mixture was neutralized with concentrated hydrochloric acid to pH 7 and evaporated under vacuum to remove methanol. The residue was adjusted to pH 3 with concentrated hydrochloric acid. The solids were collected by vacuum filtration, washed with water and dried under vacuum to give the title compound (279 mg, 87% yield) as a white solid. LC-MS (m/z) 322 (M+1).

後処理

  1. additionwas added
  2. customevaporated under vacuum
  3. customto remove methanol
  4. filtrationThe solids were collected by vacuum filtration
  5. washwashed with water
  6. customdried under vacuum

出典と根拠

ORDレコード
ord-b8e01ae05cd14242aac6a10c61d42710
出典データセット
uspto-grants-2012_05
特許番号
US08178577B2

反応ノート

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