Water → 4-[(15-Tert-butoxycarbonylpentadecanoylamino)methyl]benzoic acid

HRID 562543ノート

反応式

HRID 562543 の反応式
[NH2:1][CH2:2][C:3]1[CH:11]=[CH:10][C:6]([C:7]([OH:9])=[O:8])=[CH:5][CH:4]=1.O=C1CCC(=O)N1[O:19][C:20](=O)[CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][C:35]([O:37][C:38]([CH3:41])([CH3:40])[CH3:39])=[O:36].O>CN1C(=O)CCC1>[C:38]([O:37][C:35]([CH2:34][CH2:33][CH2:32][CH2:31][CH2:30][CH2:29][CH2:28][CH2:27][CH2:26][CH2:25][CH2:24][CH2:23][CH2:22][CH2:21][C:20]([NH:1][CH2:2][C:3]1[CH:4]=[CH:5][C:6]([C:7]([OH:9])=[O:8])=[CH:10][CH:11]=1)=[O:19])=[O:36])([CH3:41])([CH3:40])[CH3:39]

参加物

5

反応物 3

HCID 962WaterHCID 655264-(Aminomethyl)Benzoic AcidHCID 595628071-tert-Butyl 16-(2,5-dioxopyrrolidin-1-yl) hexadecanedioate

生成物 1

HCID 596879104-[(15-Tert-butoxycarbonylpentadecanoylamino)methyl]benzoic acid収率 65.8%

試薬・触媒・溶媒 1

HCID 13387N-methyl-2-pyrrolidone溶媒

実験手順

To 4-(Aminomethyl)benzoic acid (0.2 g, 1.32 mmol) was added in NMP (5 mL). Hexadecanedioic acid tert-butyl ester 2,5-dioxo-pyrrolidin-1-yl ester (0.58 g, 1.32 mmol) was added and the mixture was stirred at room temperature overnight. The mixture was poured into water (100 mL), the precipitate was isolated by filtration and dried in vacuo. The crude material was recrystallized from toluene to give 4-[(15-tert-butoxycarbonylpentadecanoylamino)methyl]benzoic acid (413 mg).

後処理

  1. customthe precipitate was isolated by filtration
  2. customdried in vacuo
  3. customThe crude material was recrystallized from toluene

出典と根拠

ORDレコード
ord-d3a1e6cf16e84016b65969a10e52caed
出典データセット
uspto-grants-2011_11
特許番号
US08067362B2

反応ノート

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