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Sodium borohydride → HCID 90449966, 화합물

HRID 1411295
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HRID 1411295 반응식
[C:1]([N:4]1[CH2:8][CH2:7][C:6]2([C:16]3[C:11](=[CH:12][CH:13]=[C:14]([CH:17]=[O:18])[CH:15]=3)[N:10]([C:19]([NH:21][C:22]3[S:23][C:24]([Cl:27])=[CH:25][N:26]=3)=[O:20])[CH2:9]2)[CH2:5]1)(=[O:3])[CH3:2].[BH4-].[Na+]>CO>[C:1]([N:4]1[CH2:8][CH2:7][C:6]2([C:16]3[C:11](=[CH:12][CH:13]=[C:14]([CH2:17][OH:18])[CH:15]=3)[N:10]([C:19]([NH:21][C:22]3[S:23][C:24]([Cl:27])=[CH:25][N:26]=3)=[O:20])[CH2:9]2)[CH2:5]1)(=[O:3])[CH3:2]
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참가 물질

4

반응물 2

HCID 4311764Sodium borohydrideHCID 90449869HCID 90449869, 화합물

생성물 1

HCID 90449966HCID 90449966, 화합물수율 99%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

The 1′-acetyl-N-(5-chlorothiazol-2-yl)-5-formylspiro[indoline-3,3′-pyrrolidine]-1-carboxamide (30.6 mg, 0.076 mmol) obtained in Step 2 of Example 401 was dissolved in methanol (1 mL). Thereafter, sodium borohydride (3.0 mg, 0.091 mmol) was added to the above obtained solution under cooling on ice, and the thus obtained mixture was then stirred at room temperature for 1 hour. Thereafter, the reaction solution was concentrated in vacuo, and the obtained residue was then purified by silica gel column chromatography (chloroform:methanol=10:1) to obtain the captioned compound (30.4 mg, 99%) in the form of a white solid.

후처리

  1. temperatureunder cooling on ice
  2. concentrationThereafter, the reaction solution was concentrated in vacuo
  3. customthe obtained residue was then purified by silica gel column chromatography (chloroform:methanol=10:1)

출처 및 근거

ORD 기록
ord-822974a0d136409db4f5f4e330b4528d
출처 데이터셋
uspto-grants-2014_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08921576B2

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