Oxalyl chloride → HCID 54351697, 화합물

HRID 2039411노트

반응식

HRID 2039411 반응식
[C:1]([OH:26])(=O)[CH2:2][CH2:3][C@H:4]([C@@H:6]1[C@:23]2([CH3:24])[C@H:9]([C@H:10]3[C@H:20]([CH2:21][CH2:22]2)[C@:18]2([CH3:19])[C@@H:13]([CH2:14][CH2:15][CH2:16][CH2:17]2)[CH2:12][CH2:11]3)[CH2:8][CH2:7]1)[CH3:5].C(Cl)(=O)C([Cl:30])=O>C(Cl)Cl>[C:1]([Cl:30])(=[O:26])[CH2:2][CH2:3][C@H:4]([C@@H:6]1[C@:23]2([CH3:24])[C@H:9]([C@H:10]3[C@H:20]([CH2:21][CH2:22]2)[C@:18]2([CH3:19])[C@@H:13]([CH2:14][CH2:15][CH2:16][CH2:17]2)[CH2:12][CH2:11]3)[CH2:8][CH2:7]1)[CH3:5]

참가 물질

4

반응물 2

HCID 65578Oxalyl chlorideHCID 92803Ursocholanic Acid

생성물 1

HCID 54351697HCID 54351697, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

반응 조건

온도
60 °C

실험 절차

A mixture of 0.5 g (1.39 mmol) of 5β-cholanic acid (Aldrich), 0.4 mL (4.6 mmol) of oxalyl chloride, and 10 mL of methylene chloride was heated in a sealed reaction vessel at 60° C. for 15 minutes. The volatiles were distilled off to give 5β-cholanoyl chloride as a colorless solid in quantitative yield. m.p. 104-106° C. 1H NMR (CDCl3, 500 MHz): δ 2.94 (m, 1H), 2.83 (m, 1H), 2.00-0.67 (m, 37H).

후처리

  1. distillationThe volatiles were distilled off

출처 및 근거

ORD 기록
ord-500083ab6a344a1997446d8df4951bd9
출처 데이터셋
uspto-grants-2013_11
특허 번호
US08580384B2

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