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Acetic Acid → Formate

HRID 82092
Notes
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Reaction equation

HRID 82092 reaction equation
Cl.[NH:2]1[CH2:5][CH2:4][CH2:3]1.[CH:6]([C:8]1[CH:9]=[C:10]([CH2:14][C:15]([NH:17][C:18]2[CH:19]=[N:20][CH:21]=[C:22]([C:24]([C:26]3[C:34]4[CH:33]=[N:32][CH:31]=[N:30][C:29]=4[N:28]([CH:35]([CH3:37])[CH3:36])[CH:27]=3)=[O:25])[CH:23]=2)=[O:16])[CH:11]=[CH:12][CH:13]=1)=O.[C:38]([OH:41])(=[O:40])C.[C:42]([O:45][BH-](OC(=O)C)OC(=O)C)(=[O:44])C.[Na+]>C(Cl)Cl.O>[CH:38]([OH:41])=[O:40].[N:2]1([CH2:6][C:8]2[CH:9]=[C:10]([CH2:14][C:15]([NH:17][C:18]3[CH:19]=[N:20][CH:21]=[C:22]([C:24]([C:26]4[C:34]5[CH:33]=[N:32][CH:31]=[N:30][C:29]=5[N:28]([CH:35]([CH3:37])[CH3:36])[CH:27]=4)=[O:25])[CH:23]=3)=[O:16])[CH:11]=[CH:12][CH:13]=2)[CH2:5][CH2:4][CH2:3]1.[CH:42]([O-:45])=[O:44]
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

8

Reactant 4

HCID 176Acetic AcidHCID 5049666Sodium triacetoxyborohydrideHCID 12308726Azetidine hydrochlorideHCID 866720722-(3-formylphenyl)-N-{5-[(7-isopropyl-7H-pyrrolo[2,3-d]pyrimidin-5-yl)carbonyl]pyridin-3-yl}acetamide

Product 2

HCID 283Formate
HCID 70817277
2-[3-(azetidin-1-ylmethyl)phenyl]-N-{5-[(7-isopropyl-7H-pyrrolo[2,3-d]pyrimidin-5-yl)carbonyl]pyridin-3-yl}acetamide formate salt

Reagents, catalysts & solvents 2

HCID 962WaterSolventHCID 6344DichloromethaneSolvent

Procedure

Azetidine hydrochloride (10 mg, 0.11 mmol) was added to a stirred solution of 2-(3-formylphenyl)-N-{5-[(7-isopropyl-7H-pyrrolo[2,3-d]pyrimidin-5-yl)carbonyl]pyridin-3-yl}acetamide (Preparation 192, 23 mg, 0.05 mmol) in DCM (1 mL) and acetic acid (0.04 mL, 0.60 mmol). The reaction mixture was stirred for 30 min at room temperature before addition of sodium triacetoxyborohydride (29 mg, 0.14 mmol) and stirring continued for 3 hours. Water (1 mL) was added and the mixture concentrated in vacuo (with toluene azeotroping). The residue was purified by preparative HPLC to afford the title compound as a formate salt in 12% yield, 3.4 mg.

Workup

  1. concentrationthe mixture concentrated in vacuo (with toluene azeotroping)
  2. customThe residue was purified by preparative HPLC

Sources & evidence

ORD record
ord-d2d80c6da06f4393a1275495ee8ff960
Source dataset
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US08846698B2

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes