Hydrochloric Acid → 2-[(2,2,2-Trifluoroacetyl)amino]hexanoic acid

HRID 1695565

반응식

HRID 1695565 반응식
[F:1][C:2]([F:8])([F:7])[C:3](OC)=[O:4].C([N:11](CC)CC)C.[CH2:16]([CH2:22][CH2:23]N)[CH2:17][CH2:18][C:19]([OH:21])=[O:20].Cl>CO.C(OCC)(=O)C>[F:8][C:2]([F:1])([F:7])[C:3]([NH:11][CH:18]([CH2:17][CH2:16][CH2:22][CH3:23])[C:19]([OH:21])=[O:20])=[O:4]

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 5646-Aminohexanoic AcidHCID 8471TriethylamineHCID 9893Methyl trifluoroacetate

생성물 1

HCID 3035902-[(2,2,2-Trifluoroacetyl)amino]hexanoic acid

시약·촉매·용매 2

HCID 887Methanol용매HCID 8857Ethyl Acetate용매

실험 절차

Methyl trifluoroacetate (513 μL, 5.10 mmoles) and triethylamine (474 μL, 3.40 mmoles) were added to a suspension of aminocaproic acid (455 mg, 3.40 mmoles) in methanol (2 mL). After the mixture was stirred vigorously for 8 h, 1 N HCl was added dropwise until the a pH of 2 was obtained. The reaction was added to ethyl acetate (10 mL) was washed with 1 N HCl (2×2 mL), dried over MgSO4, and concentrated in vacuo to yield the amide as a white solid (745 mg, 3.49 mmoles, quant.). LRMS: not performed. 1H NMR: spectrum is consistent with the predicted structure.

후처리

  1. customwas obtained
  2. washwas washed with 1 N HCl (2×2 mL)
  3. dry with materialdried over MgSO4
  4. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-fd49ac0eef1a4975958253a0d2fceec3
출처 데이터셋
uspto-grants-2012_04
특허 번호
US08163719B2

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